# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1992 data_global ########################################################################## _publ_contact_author_name 'Duan Chun-Ying' _publ_contact_author_address ; Coordination Chemistry Institute Nanjing University Nanjing 210093 P. R. China ; _publ_contact_author_email 'duancy@nju.edu.cn' _publ_contact_author_fax '86-25-3317761' _publ_contact_author_phone '86-25-3593763' _publ_requested_journal 'J. Chem. Soc., Dalton Trans' _Publ_contact_letter ; Dr. Duan Chun-ying Coordination Chemistry Institute Nanjing University, Nanjing 210093 P. R. China Date: April. 9, 2000 Dr. Debbie Middleton Editorial Secretary Dalton Transactions Dear Dr. Debbie Middleton: Our Ref: Boo1820L Title: Self-assembled dinuclear molecular box [Ag2L2]2+ and triple helicates [Co2l3]4+, [Ni2l3]4+ [ L = N,N'-bis(2-pyridylmethylene) -4,4'aminophenylether] Fellowed please find the three CIF files about the crystal structure mentioned in our paper. Questions about this manuscript, please contact me directly Thanks for your consideration With the best wishes Sincerely yours Dr. Duan Chun-Ying duancy@nju.edu.cn ; #=========================================================================== #PROCESSING SUMMARY (IUCr Office Use only) loop_ _publ_author_name _publ_author_address 'He Cheng' ; Coordination Chemistry Institute & State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, P.R. China ; 'Duan Chun-ying' ; Coordination Chemistry Institute & State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, P.R. China ; 'Fang Chen-jie' ; Coordination Chemistry Institute & State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, P.R. China ; 'Meng Qing-Jin' ; Coordination Chemistry Institute & State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, P.R. China ; ####################################################################### data_ag1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H40.50 Ag2 B2 F8 N9.50 O2' _chemical_formula_weight 1207.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.110(3) _cell_length_b 13.611(5) _cell_length_c 15.009(2) _cell_angle_alpha 105.679(13) _cell_angle_beta 92.656(18) _cell_angle_gamma 98.31(3) _cell_volume 2541.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 5.42 _cell_measurement_theta_max 9.02 _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1210 _exptl_absorpt_coefficient_mu 0.851 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 14.98 _diffrn_reflns_number 9988 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8736 _reflns_number_gt 4881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0901P)^2^+5.3765P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8736 _refine_ls_number_parameters 666 _refine_ls_number_restraints 106 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2050 _refine_ls_wR_factor_gt 0.1670 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.06439(4) 0.28061(4) 0.03029(4) 0.07150(18) Uani 1 1 d . . . N1 N 0.0504(4) 0.1312(4) 0.0864(4) 0.0591(15) Uani 1 1 d . . . N2 N 0.1921(4) 0.1917(3) -0.0263(3) 0.0474(13) Uani 1 1 d . . . N3 N 0.8780(4) 0.5389(4) -0.1201(3) 0.0505(13) Uani 1 1 d . . . N4 N 1.0736(4) 0.6385(4) -0.0383(4) 0.0608(15) Uani 1 1 d . . . O1 O 0.4696(4) 0.3508(4) -0.2416(3) 0.0805(15) Uani 1 1 d . . . C1 C -0.0168(6) 0.0967(6) 0.1372(5) 0.075(2) Uani 1 1 d . . . H1A H -0.0744 0.1292 0.1493 0.090 Uiso 1 1 calc R . . C2 C -0.0081(7) 0.0160(6) 0.1736(6) 0.087(3) Uani 1 1 d . . . H2A H -0.0578 -0.0044 0.2101 0.104 Uiso 1 1 calc R . . C3 C 0.0742(7) -0.0338(6) 0.1556(6) 0.097(3) Uani 1 1 d . . . H3A H 0.0816 -0.0896 0.1785 0.116 Uiso 1 1 calc R . . C4 C 0.1482(6) 0.0011(5) 0.1014(5) 0.077(2) Uani 1 1 d . . . H4A H 0.2068 -0.0297 0.0889 0.093 Uiso 1 1 calc R . . C5 C 0.1315(5) 0.0815(5) 0.0677(4) 0.0570(18) Uani 1 1 d . . . C6 C 0.2078(5) 0.1214(5) 0.0099(4) 0.0550(17) Uani 1 1 d . . . H6A H 0.2685 0.0935 0.0004 0.066 Uiso 1 1 calc R . . C7 C 0.2671(4) 0.2269(4) -0.0803(4) 0.0454(15) Uani 1 1 d . . . C8 C 0.2344(4) 0.2482(5) -0.1602(4) 0.0515(16) Uani 1 1 d . . . H8A H 0.1641 0.2345 -0.1793 0.062 Uiso 1 1 calc R . . C9 C 0.3018(5) 0.2888(5) -0.2124(4) 0.0573(17) Uani 1 1 d . . . H9A H 0.2775 0.3018 -0.2667 0.069 Uiso 1 1 calc R . . C10 C 0.4068(5) 0.3108(5) -0.1842(4) 0.0546(17) Uani 1 1 d . . . C11 C 0.4420(5) 0.2905(5) -0.1045(4) 0.0633(19) Uani 1 1 d . . . H11A H 0.5122 0.3056 -0.0849 0.076 Uiso 1 1 calc R . . C12 C 0.3724(5) 0.2476(5) -0.0534(4) 0.0592(18) Uani 1 1 d . . . H12A H 0.3966 0.2325 -0.0002 0.071 Uiso 1 1 calc R . . C13 C 0.5714(5) 0.3964(6) -0.2079(4) 0.069(2) Uani 1 1 d . . . C14 C 0.5949(6) 0.4976(6) -0.1569(5) 0.079(2) Uani 1 1 d . . . H14A H 0.5424 0.5365 -0.1401 0.095 Uiso 1 1 calc R . . C15 C 0.6966(5) 0.5417(6) -0.1305(5) 0.074(2) Uani 1 1 d . . . H15A H 0.7122 0.6105 -0.0955 0.088 Uiso 1 1 calc R . . C16 C 0.7747(5) 0.4872(5) -0.1542(4) 0.0508(16) Uani 1 1 d . . . C17 C 0.7520(5) 0.3854(5) -0.2074(5) 0.070(2) Uani 1 1 d . . . H17A H 0.8050 0.3474 -0.2249 0.084 Uiso 1 1 calc R . . C18 C 0.6488(6) 0.3401(6) -0.2345(5) 0.074(2) Uani 1 1 d . . . H18A H 0.6326 0.2717 -0.2705 0.089 Uiso 1 1 calc R . . C19 C 0.9547(5) 0.4905(5) -0.1296(4) 0.0584(17) Uani 1 1 d . . . H19A H 0.9433 0.4205 -0.1612 0.070 Uiso 1 1 calc R . . C20 C 1.0598(5) 0.5411(5) -0.0926(4) 0.0541(16) Uani 1 1 d . . . C21 C 1.1411(5) 0.4882(5) -0.1152(5) 0.0660(19) Uani 1 1 d . . . H21A H 1.1295 0.4202 -0.1524 0.079 Uiso 1 1 calc R . . C22 C 1.2407(6) 0.5384(7) -0.0814(6) 0.086(2) Uani 1 1 d . . . H22A H 1.2973 0.5048 -0.0959 0.103 Uiso 1 1 calc R . . C23 C 1.2539(6) 0.6368(7) -0.0271(6) 0.089(3) Uani 1 1 d . . . H23A H 1.3202 0.6717 -0.0040 0.107 Uiso 1 1 calc R . . C24 C 1.1689(6) 0.6865(6) -0.0054(5) 0.079(2) Uani 1 1 d . . . H24A H 1.1790 0.7542 0.0325 0.095 Uiso 1 1 calc R . . Ag2 Ag 0.36256(4) 0.26537(4) -0.46814(4) 0.0767(2) Uani 1 1 d . . . N5 N 0.3288(4) 0.1143(4) -0.4125(4) 0.0737(18) Uani 1 1 d . . . N6 N 0.2028(4) 0.1771(4) -0.5317(4) 0.0544(14) Uani 1 1 d . . . N7 N -0.3724(4) 0.5523(4) -0.6096(3) 0.0555(14) Uani 1 1 d . . . N8 N -0.5273(4) 0.6599(5) -0.5365(4) 0.0665(17) Uani 1 1 d . . . O2 O -0.0338(4) 0.3635(4) -0.7348(3) 0.0754(14) Uani 1 1 d . . . C25 C 0.3873(7) 0.0794(6) -0.3559(6) 0.099(3) Uani 1 1 d . . . H25B H 0.4549 0.1134 -0.3374 0.119 Uiso 1 1 calc R . . C26 C 0.3526(7) -0.0042(7) -0.3238(6) 0.101(3) Uani 1 1 d . . . H26B H 0.3958 -0.0273 -0.2858 0.121 Uiso 1 1 calc R . . C27 C 0.2542(8) -0.0511(7) -0.3493(7) 0.108(3) Uani 1 1 d . . . H27B H 0.2279 -0.1064 -0.3273 0.130 Uiso 1 1 calc R . . C28 C 0.1926(7) -0.0183(6) -0.4072(6) 0.089(3) Uani 1 1 d . . . H28B H 0.1249 -0.0518 -0.4256 0.107 Uiso 1 1 calc R . . C29 C 0.2311(5) 0.0648(5) -0.4383(5) 0.0638(19) Uani 1 1 d . . . C30 C 0.1675(5) 0.1038(5) -0.5002(5) 0.0612(19) Uani 1 1 d . . . H30B H 0.0986 0.0730 -0.5166 0.073 Uiso 1 1 calc R . . C31 C 0.1362(5) 0.2193(4) -0.5847(4) 0.0519(16) Uani 1 1 d . . . C32 C 0.0392(5) 0.2357(5) -0.5603(4) 0.0565(17) Uani 1 1 d . . . H32B H 0.0124 0.2138 -0.5113 0.068 Uiso 1 1 calc R . . C33 C -0.0187(5) 0.2849(5) -0.6087(4) 0.0593(18) Uani 1 1 d . . . H33B H -0.0845 0.2959 -0.5922 0.071 Uiso 1 1 calc R . . C34 C 0.0202(5) 0.3177(5) -0.6808(4) 0.0545(17) Uani 1 1 d . . . C35 C 0.1171(5) 0.3001(5) -0.7071(4) 0.0605(18) Uani 1 1 d . . . H35B H 0.1425 0.3200 -0.7575 0.073 Uiso 1 1 calc R . . C36 C 0.1757(5) 0.2527(5) -0.6576(4) 0.0583(18) Uani 1 1 d . . . H36B H 0.2420 0.2431 -0.6733 0.070 Uiso 1 1 calc R . . C37 C -0.1196(5) 0.4064(5) -0.6990(4) 0.0628(18) Uani 1 1 d . . . C38 C -0.2152(6) 0.3528(6) -0.7294(5) 0.076(2) Uani 1 1 d . . . H38B H -0.2239 0.2859 -0.7688 0.092 Uiso 1 1 calc R . . C39 C -0.3011(6) 0.3988(5) -0.7011(5) 0.073(2) Uani 1 1 d . . . H39B H -0.3672 0.3618 -0.7218 0.087 Uiso 1 1 calc R . . C40 C -0.2900(5) 0.4986(5) -0.6426(4) 0.0530(16) Uani 1 1 d . . . C41 C -0.1900(5) 0.5512(5) -0.6163(5) 0.067(2) Uani 1 1 d . . . H41B H -0.1796 0.6191 -0.5788 0.080 Uiso 1 1 calc R . . C42 C -0.1065(6) 0.5060(6) -0.6441(5) 0.076(2) Uani 1 1 d . . . H42B H -0.0401 0.5431 -0.6255 0.091 Uiso 1 1 calc R . . C43 C -0.4647(5) 0.5056(5) -0.6177(4) 0.0626(19) Uani 1 1 d . . . H43B H -0.4787 0.4347 -0.6455 0.075 Uiso 1 1 calc R . . C44 C -0.5497(5) 0.5600(5) -0.5844(4) 0.0552(17) Uani 1 1 d . . . C45 C -0.6503(6) 0.5065(6) -0.6044(5) 0.080(2) Uani 1 1 d . . . H45B H -0.6629 0.4367 -0.6369 0.095 Uiso 1 1 calc R . . C46 C -0.7302(6) 0.5575(7) -0.5757(5) 0.088(3) Uani 1 1 d . . . H46B H -0.7981 0.5230 -0.5889 0.106 Uiso 1 1 calc R . . C47 C -0.7096(6) 0.6608(8) -0.5270(6) 0.100(3) Uani 1 1 d . . . H47B H -0.7624 0.6979 -0.5066 0.120 Uiso 1 1 calc R . . C48 C -0.6053(6) 0.7070(7) -0.5097(5) 0.085(3) Uani 1 1 d . . . H48B H -0.5904 0.7765 -0.4765 0.102 Uiso 1 1 calc R . . N9 N 0.6399(9) 0.1252(9) -0.1572(9) 0.177(4) Uani 1 1 d U . . C49 C 0.6537(12) 0.0691(12) -0.2326(12) 0.180(5) Uani 1 1 d U . . C50 C 0.6721(12) 0.0090(12) -0.3205(10) 0.204(6) Uani 1 1 d U . . H50C H 0.6447 0.0362 -0.3676 0.245 Uiso 1 1 d R . . H50A H 0.6381 -0.0610 -0.3308 0.245 Uiso 1 1 d R . . H50B H 0.7448 0.0093 -0.3261 0.245 Uiso 1 1 d R . . B1 B 0.4441(14) 0.2152(14) 0.2149(12) 0.150(4) Uani 1 1 d U . . F11 F 0.4940(6) 0.2611(6) 0.1595(5) 0.173(3) Uani 1 1 d U A . F12 F 0.3607(9) 0.1439(9) 0.1698(7) 0.148(4) Uiso 0.650(7) 1 d PU A 1 F13 F 0.4335(8) 0.2606(8) 0.3000(7) 0.142(3) Uiso 0.650(7) 1 d PU A 1 F14 F 0.5278(10) 0.1578(10) 0.2267(9) 0.173(4) Uiso 0.650(7) 1 d PU A 1 F12' F 0.4027(19) 0.1056(18) 0.1602(15) 0.162(6) Uiso 0.350(7) 1 d PU A 2 F13' F 0.3820(19) 0.2816(18) 0.2255(16) 0.174(6) Uiso 0.350(7) 1 d PU A 2 F14' F 0.4809(18) 0.1926(18) 0.2900(16) 0.163(6) Uiso 0.350(7) 1 d PU A 2 B2 B 0.9572(9) 0.2109(8) 0.6788(8) 0.098(2) Uani 1 1 d U . . F21 F 0.9514(5) 0.2343(4) 0.7671(3) 0.130(2) Uani 1 1 d U B . F22 F 1.0641(7) 0.2474(7) 0.6684(6) 0.124(3) Uiso 0.628(6) 1 d PU B 1 F23 F 0.9494(9) 0.1068(9) 0.6343(8) 0.141(3) Uiso 0.628(6) 1 d PU B 1 F24 F 0.9002(8) 0.2417(8) 0.6192(7) 0.121(3) Uiso 0.628(6) 1 d PU B 1 F22' F 0.8479(16) 0.1528(15) 0.6699(13) 0.155(5) Uiso 0.372(6) 1 d PU B 2 F23' F 0.9325(10) 0.2916(10) 0.6416(8) 0.081(3) Uiso 0.372(6) 1 d PU B 2 F24' F 1.0040(15) 0.1260(15) 0.6413(13) 0.136(5) Uiso 0.372(6) 1 d PU B 2 C51 C 0.6489(18) 0.0873(17) 0.0684(15) 0.122(7) Uiso 0.50 1 d PU . . N10 N 0.7057(15) 0.1017(14) 0.1095(13) 0.125(6) Uiso 0.50 1 d PU . . C52 C 0.546(2) 0.045(3) 0.019(2) 0.210(14) Uiso 0.50 1 d P . . H52A H 0.5358 0.0709 -0.0337 0.315 Uiso 0.50 1 d PR . . H52B H 0.5400 -0.0288 -0.0013 0.315 Uiso 0.50 1 d PR . . H52C H 0.4953 0.0643 0.0615 0.315 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0643(3) 0.0636(3) 0.0915(4) 0.0221(3) 0.0115(3) 0.0241(3) N1 0.054(3) 0.051(3) 0.065(3) 0.012(3) 0.008(3) -0.005(2) N2 0.046(3) 0.044(3) 0.053(3) 0.015(2) 0.005(2) 0.004(2) N3 0.047(3) 0.050(3) 0.057(3) 0.021(2) 0.012(2) 0.003(2) N4 0.059(3) 0.064(3) 0.062(3) 0.022(3) 0.004(3) 0.012(3) O1 0.057(3) 0.122(4) 0.066(3) 0.047(3) 0.001(2) -0.012(3) C1 0.069(5) 0.081(5) 0.068(4) 0.018(4) 0.014(4) -0.005(4) C2 0.084(5) 0.086(5) 0.081(5) 0.027(4) 0.008(4) -0.025(5) C3 0.108(7) 0.087(5) 0.107(6) 0.061(5) 0.012(5) -0.006(5) C4 0.082(5) 0.064(4) 0.095(5) 0.038(4) 0.008(4) 0.014(4) C5 0.055(4) 0.053(4) 0.058(4) 0.015(3) -0.005(3) -0.002(3) C6 0.047(3) 0.048(3) 0.072(4) 0.021(3) 0.007(3) 0.009(3) C7 0.042(3) 0.048(3) 0.049(3) 0.015(3) 0.004(3) 0.014(3) C8 0.038(3) 0.056(3) 0.062(4) 0.017(3) 0.009(3) 0.007(3) C9 0.059(4) 0.063(4) 0.055(4) 0.027(3) -0.006(3) 0.009(3) C10 0.047(3) 0.069(4) 0.049(3) 0.025(3) 0.004(3) -0.002(3) C11 0.035(3) 0.099(5) 0.062(4) 0.035(4) -0.004(3) 0.005(3) C12 0.042(3) 0.086(4) 0.055(4) 0.032(3) -0.002(3) 0.008(3) C13 0.058(4) 0.097(5) 0.054(4) 0.034(4) 0.009(3) -0.004(4) C14 0.056(4) 0.094(6) 0.080(5) 0.006(4) 0.011(4) 0.018(4) C15 0.057(4) 0.074(5) 0.078(5) 0.002(4) 0.005(4) 0.010(4) C16 0.053(3) 0.053(3) 0.053(3) 0.026(3) 0.016(3) 0.004(3) C17 0.050(4) 0.054(4) 0.104(5) 0.021(4) 0.008(4) 0.001(3) C18 0.073(5) 0.061(4) 0.085(5) 0.021(4) -0.004(4) 0.004(4) C19 0.062(4) 0.053(3) 0.067(4) 0.026(3) 0.012(3) 0.015(3) C20 0.056(4) 0.055(3) 0.061(4) 0.028(3) 0.010(3) 0.015(3) C21 0.060(4) 0.070(4) 0.072(4) 0.019(3) 0.008(3) 0.023(3) C22 0.069(5) 0.108(6) 0.093(6) 0.038(5) 0.008(4) 0.036(4) C23 0.049(4) 0.098(6) 0.117(7) 0.024(5) -0.009(4) 0.019(4) C24 0.069(5) 0.072(5) 0.092(5) 0.020(4) -0.006(4) 0.011(4) Ag2 0.0513(3) 0.0674(4) 0.1003(4) 0.0161(3) -0.0051(3) -0.0080(3) N5 0.060(3) 0.057(3) 0.098(4) 0.017(3) -0.012(3) 0.001(3) N6 0.044(3) 0.054(3) 0.062(3) 0.015(2) -0.001(2) 0.002(2) N7 0.056(3) 0.057(3) 0.055(3) 0.027(2) -0.011(2) -0.004(2) N8 0.047(3) 0.081(4) 0.061(3) 0.010(3) 0.000(3) -0.004(3) O2 0.079(3) 0.100(3) 0.063(3) 0.037(2) 0.014(2) 0.033(3) C25 0.077(5) 0.081(5) 0.135(7) 0.027(5) -0.035(5) 0.025(4) C26 0.109(7) 0.089(5) 0.123(7) 0.058(5) -0.014(5) 0.028(5) C27 0.114(7) 0.095(5) 0.139(7) 0.078(5) -0.005(6) 0.012(5) C28 0.084(5) 0.078(5) 0.113(6) 0.053(4) -0.008(5) -0.004(4) C29 0.062(4) 0.051(4) 0.073(4) 0.009(3) -0.009(3) 0.011(3) C30 0.049(4) 0.053(4) 0.073(4) 0.011(3) -0.007(3) -0.002(3) C31 0.051(3) 0.045(3) 0.055(4) 0.012(3) 0.000(3) -0.003(3) C32 0.046(3) 0.075(4) 0.053(4) 0.027(3) 0.014(3) 0.006(3) C33 0.044(3) 0.077(4) 0.057(4) 0.020(3) -0.003(3) 0.012(3) C34 0.058(4) 0.059(4) 0.042(3) 0.013(3) -0.001(3) -0.002(3) C35 0.067(4) 0.066(4) 0.049(4) 0.021(3) 0.015(3) 0.000(3) C36 0.045(3) 0.066(4) 0.059(4) 0.014(3) 0.010(3) -0.001(3) C37 0.066(4) 0.079(4) 0.051(4) 0.033(3) 0.001(3) 0.009(4) C38 0.080(5) 0.068(4) 0.079(5) 0.019(4) 0.003(4) 0.011(4) C39 0.065(4) 0.060(4) 0.081(5) 0.010(4) -0.013(4) -0.007(4) C40 0.051(3) 0.048(3) 0.060(4) 0.020(3) -0.012(3) 0.006(3) C41 0.053(4) 0.058(4) 0.079(5) 0.008(4) -0.005(3) 0.000(3) C42 0.052(4) 0.084(5) 0.084(5) 0.015(4) -0.009(4) 0.008(4) C43 0.068(4) 0.051(4) 0.068(4) 0.026(3) -0.003(3) -0.006(3) C44 0.052(4) 0.071(4) 0.049(3) 0.032(3) 0.004(3) -0.001(3) C45 0.057(4) 0.101(5) 0.082(5) 0.046(4) -0.001(4) -0.018(4) C46 0.064(5) 0.123(7) 0.072(5) 0.034(5) 0.005(4) -0.018(5) C47 0.046(4) 0.156(8) 0.101(6) 0.032(6) 0.024(4) 0.024(5) C48 0.067(5) 0.102(6) 0.068(5) -0.007(4) 0.012(4) 0.014(4) N9 0.169(8) 0.140(7) 0.228(10) 0.049(7) 0.015(8) 0.052(7) C49 0.175(9) 0.154(9) 0.219(11) 0.042(8) 0.026(9) 0.065(8) C50 0.196(11) 0.185(11) 0.203(12) -0.017(10) 0.070(10) 0.060(9) B1 0.139(6) 0.160(6) 0.149(6) 0.052(5) 0.010(6) 0.002(6) F11 0.158(6) 0.207(6) 0.148(5) 0.079(5) -0.032(4) -0.035(5) B2 0.125(5) 0.093(4) 0.100(5) 0.051(4) 0.034(4) 0.044(4) F21 0.222(6) 0.099(3) 0.084(3) 0.030(3) 0.029(4) 0.062(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.242(5) 2_665 ? Ag1 N2 2.270(5) . ? Ag1 N1 2.390(6) . ? Ag1 N3 2.450(5) 2_665 ? N1 C1 1.309(9) . ? N1 C5 1.340(8) . ? N2 C6 1.257(8) . ? N2 C7 1.415(7) . ? N3 C19 1.271(8) . ? N3 C16 1.435(7) . ? N3 Ag1 2.450(5) 2_665 ? N4 C24 1.328(9) . ? N4 C20 1.337(8) . ? N4 Ag1 2.242(5) 2_665 ? O1 C10 1.380(7) . ? O1 C13 1.396(8) . ? C1 C2 1.369(11) . ? C2 C3 1.355(12) . ? C3 C4 1.406(11) . ? C4 C5 1.364(10) . ? C5 C6 1.492(9) . ? C7 C8 1.371(8) . ? C7 C12 1.386(8) . ? C8 C9 1.363(9) . ? C9 C10 1.386(8) . ? C10 C11 1.373(9) . ? C11 C12 1.384(9) . ? C13 C14 1.366(10) . ? C13 C18 1.368(10) . ? C14 C15 1.373(10) . ? C15 C16 1.355(9) . ? C16 C17 1.381(8) . ? C17 C18 1.397(9) . ? C19 C20 1.459(9) . ? C20 C21 1.376(9) . ? C21 C22 1.387(10) . ? C22 C23 1.349(11) . ? C23 C24 1.391(10) . ? Ag2 N8 2.240(5) 2_564 ? Ag2 N6 2.282(5) . ? Ag2 N5 2.413(6) . ? Ag2 N7 2.421(5) 2_564 ? N5 C25 1.341(10) . ? N5 C29 1.344(8) . ? N6 C30 1.255(8) . ? N6 C31 1.432(8) . ? N7 C43 1.267(8) . ? N7 C40 1.424(8) . ? N7 Ag2 2.421(5) 2_564 ? N8 C48 1.307(9) . ? N8 C44 1.337(8) . ? N8 Ag2 2.240(5) 2_564 ? O2 C34 1.377(8) . ? O2 C37 1.404(8) . ? C25 C26 1.378(12) . ? C26 C27 1.342(12) . ? C27 C28 1.362(12) . ? C28 C29 1.377(10) . ? C29 C30 1.471(9) . ? C31 C32 1.373(9) . ? C31 C36 1.387(9) . ? C32 C33 1.383(9) . ? C33 C34 1.369(9) . ? C34 C35 1.382(9) . ? C35 C36 1.381(9) . ? C37 C38 1.347(10) . ? C37 C42 1.365(10) . ? C38 C39 1.395(10) . ? C39 C40 1.387(9) . ? C40 C41 1.384(8) . ? C41 C42 1.359(10) . ? C43 C44 1.459(9) . ? C44 C45 1.388(9) . ? C45 C46 1.362(11) . ? C46 C47 1.378(12) . ? C47 C48 1.402(11) . ? N9 C49 1.220(18) . ? C49 C50 1.404(19) . ? B1 F13 1.283(19) . ? B1 F13' 1.29(3) . ? B1 F11 1.313(18) . ? B1 F14' 1.33(3) . ? B1 F12 1.365(18) . ? B1 F14 1.47(2) . ? B1 F12' 1.50(3) . ? B2 F21 1.286(11) . ? B2 F24 1.330(14) . ? B2 F23 1.379(14) . ? B2 F24' 1.38(2) . ? B2 F23' 1.428(16) . ? B2 F22 1.448(14) . ? B2 F22' 1.51(2) . ? C51 N10 0.91(3) . ? C51 C52 1.46(3) . ? C52 C52 1.56(6) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N2 161.88(18) 2_665 . ? N4 Ag1 N1 116.89(19) 2_665 . ? N2 Ag1 N1 72.44(18) . . ? N4 Ag1 N3 72.50(18) 2_665 2_665 ? N2 Ag1 N3 115.42(16) . 2_665 ? N1 Ag1 N3 127.31(17) . 2_665 ? C1 N1 C5 116.9(6) . . ? C1 N1 Ag1 131.0(5) . . ? C5 N1 Ag1 111.9(4) . . ? C6 N2 C7 119.4(5) . . ? C6 N2 Ag1 115.6(4) . . ? C7 N2 Ag1 123.1(4) . . ? C19 N3 C16 121.6(5) . . ? C19 N3 Ag1 109.9(4) . 2_665 ? C16 N3 Ag1 128.4(4) . 2_665 ? C24 N4 C20 119.2(6) . . ? C24 N4 Ag1 123.5(5) . 2_665 ? C20 N4 Ag1 116.3(4) . 2_665 ? C10 O1 C13 118.8(5) . . ? N1 C1 C2 124.4(8) . . ? C3 C2 C1 118.9(8) . . ? C2 C3 C4 118.4(8) . . ? C5 C4 C3 118.0(8) . . ? N1 C5 C4 123.4(7) . . ? N1 C5 C6 116.6(6) . . ? C4 C5 C6 120.0(6) . . ? N2 C6 C5 121.6(6) . . ? C8 C7 C12 117.9(6) . . ? C8 C7 N2 118.8(5) . . ? C12 C7 N2 123.1(5) . . ? C9 C8 C7 122.1(6) . . ? C8 C9 C10 119.6(6) . . ? C11 C10 O1 124.4(5) . . ? C11 C10 C9 119.7(6) . . ? O1 C10 C9 115.9(5) . . ? C10 C11 C12 119.7(6) . . ? C11 C12 C7 121.0(6) . . ? C14 C13 C18 120.2(7) . . ? C14 C13 O1 121.3(7) . . ? C18 C13 O1 118.3(6) . . ? C13 C14 C15 119.5(7) . . ? C16 C15 C14 121.6(7) . . ? C15 C16 C17 119.5(6) . . ? C15 C16 N3 117.3(5) . . ? C17 C16 N3 123.2(6) . . ? C16 C17 C18 119.2(7) . . ? C13 C18 C17 120.0(7) . . ? N3 C19 C20 122.3(6) . . ? N4 C20 C21 122.2(6) . . ? N4 C20 C19 118.3(6) . . ? C21 C20 C19 119.5(6) . . ? C20 C21 C22 118.7(7) . . ? C23 C22 C21 118.6(7) . . ? C22 C23 C24 120.4(7) . . ? N4 C24 C23 120.8(7) . . ? N8 Ag2 N6 158.09(19) 2_564 . ? N8 Ag2 N5 118.2(2) 2_564 . ? N6 Ag2 N5 71.96(19) . . ? N8 Ag2 N7 72.8(2) 2_564 2_564 ? N6 Ag2 N7 116.38(18) . 2_564 ? N5 Ag2 N7 131.60(19) . 2_564 ? C25 N5 C29 117.7(7) . . ? C25 N5 Ag2 130.7(5) . . ? C29 N5 Ag2 111.4(5) . . ? C30 N6 C31 120.7(5) . . ? C30 N6 Ag2 116.1(4) . . ? C31 N6 Ag2 121.2(4) . . ? C43 N7 C40 121.4(5) . . ? C43 N7 Ag2 110.6(4) . 2_564 ? C40 N7 Ag2 127.9(4) . 2_564 ? C48 N8 C44 116.9(6) . . ? C48 N8 Ag2 126.4(5) . 2_564 ? C44 N8 Ag2 115.8(4) . 2_564 ? C34 O2 C37 117.7(5) . . ? N5 C25 C26 123.4(8) . . ? C27 C26 C25 117.8(8) . . ? C26 C27 C28 120.5(8) . . ? C27 C28 C29 119.6(8) . . ? N5 C29 C28 121.0(7) . . ? N5 C29 C30 117.3(6) . . ? C28 C29 C30 121.7(6) . . ? N6 C30 C29 122.3(6) . . ? C32 C31 C36 119.6(6) . . ? C32 C31 N6 122.0(6) . . ? C36 C31 N6 118.1(6) . . ? C31 C32 C33 119.8(6) . . ? C34 C33 C32 120.5(6) . . ? C33 C34 O2 124.2(6) . . ? C33 C34 C35 120.3(6) . . ? O2 C34 C35 115.4(6) . . ? C36 C35 C34 119.2(6) . . ? C35 C36 C31 120.5(6) . . ? C38 C37 C42 120.6(7) . . ? C38 C37 O2 118.8(6) . . ? C42 C37 O2 120.0(6) . . ? C37 C38 C39 119.3(7) . . ? C40 C39 C38 121.3(6) . . ? C41 C40 C39 116.8(6) . . ? C41 C40 N7 117.4(5) . . ? C39 C40 N7 125.7(6) . . ? C42 C41 C40 121.6(6) . . ? C41 C42 C37 120.4(7) . . ? N7 C43 C44 121.9(6) . . ? N8 C44 C45 122.8(7) . . ? N8 C44 C43 118.4(6) . . ? C45 C44 C43 118.8(6) . . ? C46 C45 C44 119.1(8) . . ? C45 C46 C47 119.5(7) . . ? C46 C47 C48 116.7(8) . . ? N8 C48 C47 125.0(8) . . ? N9 C49 C50 177.1(18) . . ? F13 B1 F13' 65.8(15) . . ? F13 B1 F11 123.6(15) . . ? F13' B1 F11 89.0(17) . . ? F13 B1 F14' 53.0(13) . . ? F13' B1 F14' 118(2) . . ? F11 B1 F14' 129.1(18) . . ? F13 B1 F12 114.5(15) . . ? F13' B1 F12 86.0(16) . . ? F11 B1 F12 112.8(14) . . ? F14' B1 F12 111.3(17) . . ? F13 B1 F14 100.6(14) . . ? F13' B1 F14 164.6(19) . . ? F11 B1 F14 93.3(13) . . ? F14' B1 F14 49.7(13) . . ? F12 B1 F14 107.0(15) . . ? F13 B1 F12' 128.4(17) . . ? F13' B1 F12' 118.0(19) . . ? F11 B1 F12' 108.0(15) . . ? F14' B1 F12' 96.2(18) . . ? F12 B1 F12' 32.1(11) . . ? F14 B1 F12' 75.7(14) . . ? F21 B2 F24 125.2(10) . . ? F21 B2 F23 115.8(10) . . ? F24 B2 F23 101.4(10) . . ? F21 B2 F24' 116.0(12) . . ? F24 B2 F24' 116.2(12) . . ? F23 B2 F24' 30.2(9) . . ? F21 B2 F23' 111.2(9) . . ? F24 B2 F23' 30.4(6) . . ? F23 B2 F23' 128.5(11) . . ? F24' B2 F23' 131.3(13) . . ? F21 B2 F22 104.5(9) . . ? F24 B2 F22 106.3(10) . . ? F23 B2 F22 100.9(10) . . ? F24' B2 F22 71.6(10) . . ? F23' B2 F22 86.3(9) . . ? F21 B2 F22' 86.5(10) . . ? F24 B2 F22' 72.0(11) . . ? F23 B2 F22' 67.1(10) . . ? F24' B2 F22' 97.0(13) . . ? F23' B2 F22' 96.8(12) . . ? F22 B2 F22' 166.8(12) . . ? N10 C51 C52 163(3) . . ? C51 C52 C52 152(4) . 2_655 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.620 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.090 #### END of this CIF #### ###################################################################### data_Co1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C74.50 H59 B4 Co2 F16 N13 O3.50' _chemical_formula_weight 1657.45 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'Cc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.780(4) _cell_length_b 18.385(3) _cell_length_c 20.144(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.93(2) _cell_angle_gamma 90.00 _cell_volume 7769.8(29) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 5.41 _cell_measurement_theta_max 9.64 _exptl_crystal_description 'prism ' _exptl_crystal_colour 'orange ' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method ? _exptl_crystal_F_000 3372 _exptl_absorpt_coefficient_mu 0.522 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 11.36 _diffrn_reflns_number 7817 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.1172 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 24.99 _reflns_number_total 7319 _reflns_number_observed 3413 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 7310 _refine_ls_number_parameters 1196 _refine_ls_number_restraints 400 _refine_ls_R_factor_all 0.1781 _refine_ls_R_factor_obs 0.0772 _refine_ls_wR_factor_all 0.2185 _refine_ls_wR_factor_obs 0.1606 _refine_ls_goodness_of_fit_all 1.083 _refine_ls_goodness_of_fit_obs 1.316 _refine_ls_restrained_S_all 1.074 _refine_ls_restrained_S_obs 1.238 _refine_ls_shift/esd_max -0.013 _refine_ls_shift/esd_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co -0.24308(6) -0.19101(6) -0.18072(6) 0.0667(4) Uani 1 d . . Co2 Co 0.13859(6) 0.17619(7) 0.20765(6) 0.0717(4) Uani 1 d . . O1 O 0.0296(3) -0.1892(3) 0.1433(3) 0.097(3) Uani 1 d . . O2 O -0.0076(3) 0.0692(3) -0.1642(3) 0.099(2) Uani 1 d . . O3 O -0.1944(3) 0.1481(3) 0.0051(3) 0.082(2) Uani 1 d . . N1 N -0.3317(4) -0.2044(4) -0.1730(4) 0.075(3) Uani 1 d . . N2 N -0.2159(3) -0.2014(3) -0.0680(3) 0.067(2) Uani 1 d . . N3 N 0.1668(3) 0.0678(4) 0.1855(3) 0.066(2) Uani 1 d . . N4 N 0.2321(4) 0.1972(5) 0.2075(4) 0.091(3) Uani 1 d . . N5 N -0.2131(3) -0.3022(4) -0.1829(3) 0.072(2) Uani 1 d . . N6 N -0.1503(3) -0.1803(4) -0.1826(3) 0.067(2) Uani 1 d . . N7 N 0.0846(3) 0.2154(4) 0.0994(4) 0.068(2) Uani 1 d . . N8 N 0.1219(3) 0.2866(4) 0.2246(3) 0.075(3) Uani 1 d . . N9 N -0.2857(4) -0.1812(4) -0.2952(4) 0.081(3) Uani 1 d . . N10 N -0.2618(3) -0.0756(4) -0.1983(4) 0.075(2) Uani 1 d . . N11 N 0.0517(3) 0.1450(3) 0.2194(3) 0.057(2) Uani 1 d . . N12 N 0.1703(3) 0.1533(4) 0.3197(3) 0.068(2) Uani 1 d . . C1 C -0.3896(5) -0.2034(5) -0.2235(5) 0.090(4) Uani 1 d . . H1A H -0.3940(5) -0.2011(5) -0.2713(5) 0.108 Uiso 1 calc R . C2 C -0.4449(5) -0.2058(6) -0.2091(6) 0.095(4) Uani 1 d . . H2A H -0.4843(5) -0.2008(6) -0.2472(6) 0.114 Uiso 1 calc R . C3 C -0.4434(5) -0.2146(5) -0.1448(6) 0.096(4) Uani 1 d . . H3A H -0.4801(5) -0.2205(5) -0.1355(6) 0.115 Uiso 1 calc R . C4 C -0.3813(5) -0.2146(5) -0.0895(5) 0.088(3) Uani 1 d . . H4A H -0.3766(5) -0.2164(5) -0.0415(5) 0.105 Uiso 1 calc R . C5 C -0.3292(5) -0.2121(5) -0.1054(5) 0.075(3) Uani 1 d . . C6 C -0.2618(5) -0.2118(4) -0.0506(5) 0.072(3) Uani 1 d . . H6A H -0.2542(5) -0.2196(4) -0.0024(5) 0.086 Uiso 1 calc R . C7 C -0.1542(4) -0.1985(4) -0.0109(4) 0.068(3) Uani 1 d . . C8 C -0.1084(5) -0.2516(5) -0.0032(5) 0.107(4) Uani 1 d . . H8A H -0.1191(5) -0.2909(5) -0.0348(5) 0.128 Uiso 1 calc R . C9 C -0.0493(6) -0.2480(6) 0.0484(5) 0.117(5) Uani 1 d . . H9A H -0.0209(6) -0.2862(6) 0.0543(5) 0.140 Uiso 1 calc R . C10 C -0.0317(5) -0.1905(5) 0.0904(4) 0.080(3) Uani 1 d . . C11 C -0.0744(6) -0.1345(6) 0.0836(7) 0.137(6) Uani 1 d . . H11A H -0.0615(6) -0.0938(6) 0.1131(7) 0.164 Uiso 1 calc R . C12 C -0.1360(5) -0.1393(5) 0.0332(6) 0.113(5) Uani 1 d . . H12A H -0.1650(5) -0.1023(5) 0.0292(6) 0.136 Uiso 1 calc R . C13 C 0.0624(5) -0.1258(5) 0.1534(5) 0.082(3) Uani 1 d . . C14 C 0.0804(5) -0.0975(6) 0.0984(5) 0.105(4) Uani 1 d . . H14A H 0.0697(5) -0.1221(6) 0.0549(5) 0.126 Uiso 1 calc R . C15 C 0.1126(5) -0.0356(5) 0.1098(5) 0.092(4) Uani 1 d . . H15A H 0.1236(5) -0.0172(5) 0.0731(5) 0.111 Uiso 1 calc R . C16 C 0.1306(4) 0.0024(5) 0.1731(4) 0.066(3) Uani 1 d . . C17 C 0.1143(4) -0.0234(5) 0.2268(4) 0.074(3) Uani 1 d . . H17A H 0.1262(4) 0.0016(5) 0.2702(4) 0.089 Uiso 1 calc R . C18 C 0.0788(4) -0.0891(5) 0.2160(5) 0.078(3) Uani 1 d . . H18A H 0.0669(4) -0.1067(5) 0.2522(5) 0.094 Uiso 1 calc R . C19 C 0.2205(5) 0.0674(5) 0.1799(5) 0.081(3) Uani 1 d . . H19A H 0.2362(5) 0.0246(5) 0.1683(5) 0.097 Uiso 1 calc R . C20 C 0.2582(5) 0.1361(6) 0.1919(5) 0.092(4) Uani 1 d . . C21 C 0.3155(5) 0.1373(9) 0.1847(7) 0.138(5) Uani 1 d . . H21A H 0.3326(5) 0.0953(9) 0.1736(7) 0.165 Uiso 1 calc R . C22 C 0.3480(6) 0.2048(10) 0.1949(8) 0.170(7) Uani 1 d . . H22A H 0.3864(6) 0.2091(10) 0.1891(8) 0.204 Uiso 1 calc R . C23 C 0.3213(6) 0.2626(9) 0.2134(7) 0.152(6) Uani 1 d . . H23A H 0.3439(6) 0.3061(9) 0.2247(7) 0.182 Uiso 1 calc R . C24 C 0.2641(5) 0.2601(7) 0.2163(6) 0.111(4) Uani 1 d . . H24A H 0.2459(5) 0.3027(7) 0.2245(6) 0.133 Uiso 1 calc R . C25 C -0.2433(6) -0.3627(4) -0.1739(5) 0.084(3) Uani 1 d . . H25A H -0.2814(6) -0.3575(4) -0.1675(5) 0.101 Uiso 1 calc R . C26 C -0.2198(6) -0.4304(5) -0.1739(5) 0.103(4) Uani 1 d . . H26A H -0.2418(6) -0.4715(5) -0.1695(5) 0.124 Uiso 1 calc R . C27 C -0.1605(6) -0.4364(6) -0.1809(6) 0.115(5) Uani 1 d . . H27A H -0.1431(6) -0.4821(6) -0.1812(6) 0.138 Uiso 1 calc R . C28 C -0.1291(6) -0.3763(5) -0.1871(7) 0.126(5) Uani 1 d . . H28A H -0.0899(6) -0.3800(5) -0.1909(7) 0.151 Uiso 1 calc R . C29 C -0.1568(5) -0.3078(5) -0.1875(5) 0.082(3) Uani 1 d . . C30 C -0.1259(5) -0.2414(5) -0.1923(5) 0.084(3) Uani 1 d . . H30A H -0.0893(5) -0.2420(5) -0.2021(5) 0.101 Uiso 1 calc R . C31 C -0.1146(4) -0.1159(4) -0.1795(4) 0.063(3) Uani 1 d . . C32 C -0.1189(4) -0.0793(5) -0.2389(5) 0.081(3) Uani 1 d . . H32A H -0.1447(4) -0.0967(5) -0.2842(5) 0.097 Uiso 1 calc R . C33 C -0.0843(4) -0.0150(6) -0.2321(4) 0.085(3) Uani 1 d . . H33A H -0.0895(4) 0.0119(6) -0.2731(4) 0.101 Uiso 1 calc R . C34 C -0.0423(4) 0.0093(5) -0.1654(4) 0.069(3) Uani 1 d . . C35 C -0.0392(5) -0.0294(5) -0.1056(5) 0.097(4) Uani 1 d . . H35A H -0.0126(5) -0.0138(5) -0.0598(5) 0.116 Uiso 1 calc R . C36 C -0.0749(5) -0.0901(5) -0.1136(5) 0.091(4) Uani 1 d . . H36A H -0.0723(5) -0.1153(5) -0.0726(5) 0.110 Uiso 1 calc R . C37 C 0.0159(5) 0.1061(5) -0.0970(5) 0.082(3) Uani 1 d . . C38 C -0.0269(5) 0.1488(6) -0.0782(5) 0.091(4) Uani 1 d . . H38A H -0.0695(5) 0.1536(6) -0.1090(5) 0.110 Uiso 1 calc R . C39 C -0.0033(4) 0.1820(5) -0.0143(5) 0.080(3) Uani 1 d . . H39A H -0.0306(4) 0.2092(5) 0.0003(5) 0.096 Uiso 1 calc R . C40 C 0.0607(4) 0.1772(5) 0.0313(5) 0.074(3) Uani 1 d . . C41 C 0.1013(5) 0.1374(5) 0.0111(5) 0.087(3) Uani 1 d . . H41A H 0.1442(5) 0.1350(5) 0.0411(5) 0.104 Uiso 1 calc R . C42 C 0.0794(5) 0.1012(5) -0.0527(5) 0.094(4) Uani 1 d . . H42A H 0.1070(5) 0.0735(5) -0.0662(5) 0.113 Uiso 1 calc R . C43 C 0.0662(5) 0.2815(5) 0.0985(5) 0.082(3) Uani 1 d . . H43A H 0.0410(5) 0.3033(5) 0.0551(5) 0.099 Uiso 1 calc R . C44 C 0.0847(4) 0.3219(5) 0.1652(5) 0.076(3) Uani 1 d . . C45 C 0.0645(6) 0.3922(6) 0.1665(6) 0.112(4) Uani 1 d . . H45A H 0.0390(6) 0.4151(6) 0.1238(6) 0.135 Uiso 1 calc R . C46 C 0.0825(6) 0.4293(6) 0.2326(6) 0.124(5) Uani 1 d . . H46A H 0.0707(6) 0.4772(6) 0.2356(6) 0.149 Uiso 1 calc R . C47 C 0.1195(5) 0.3886(6) 0.2936(6) 0.105(4) Uani 1 d . . H47A H 0.1312(5) 0.4092(6) 0.3391(6) 0.126 Uiso 1 calc R . C48 C 0.1385(5) 0.3199(6) 0.2876(5) 0.098(4) Uani 1 d . . H48A H 0.1642(5) 0.2953(6) 0.3292(5) 0.117 Uiso 1 calc R . C49 C -0.2927(5) -0.2360(6) -0.3419(5) 0.090(4) Uani 1 d . . H49A H -0.2823(5) -0.2829(6) -0.3239(5) 0.108 Uiso 1 calc R . C50 C -0.3141(7) -0.2259(7) -0.4133(6) 0.141(6) Uani 1 d . . H50A H -0.3177(7) -0.2640(7) -0.4450(6) 0.169 Uiso 1 calc R . C51 C -0.3309(9) -0.1530(10) -0.4375(7) 0.209(10) Uani 1 d . . H51A H -0.3474(9) -0.1429(10) -0.4866(7) 0.251 Uiso 1 calc R . C52 C -0.3232(8) -0.0982(6) -0.3896(5) 0.145(6) Uani 1 d . . H52A H -0.3344(8) -0.0507(6) -0.4054(5) 0.174 Uiso 1 calc R . C53 C -0.2993(5) -0.1139(5) -0.3196(5) 0.091(4) Uani 1 d . . C54 C -0.2874(5) -0.0599(5) -0.2665(5) 0.086(4) Uani 1 d . . H54A H -0.2981(5) -0.0119(5) -0.2806(5) 0.104 Uiso 1 calc R . C55 C -0.2479(4) -0.0153(4) -0.1477(4) 0.062(3) Uani 1 d . . C56 C -0.2159(4) 0.0439(5) -0.1577(5) 0.073(3) Uani 1 d . . H56A H -0.2057(4) 0.0471(5) -0.1980(5) 0.087 Uiso 1 calc R . C57 C -0.1985(4) 0.1000(5) -0.1055(5) 0.078(3) Uani 1 d . . H57A H -0.1778(4) 0.1413(5) -0.1122(5) 0.093 Uiso 1 calc R . C58 C -0.2118(4) 0.0939(5) -0.0460(5) 0.069(3) Uani 1 d . . C59 C -0.2454(4) 0.0349(5) -0.0376(5) 0.069(3) Uani 1 d . . H59A H -0.2573(4) 0.0327(5) 0.0016(5) 0.083 Uiso 1 calc R . C60 C -0.2617(4) -0.0216(5) -0.0876(4) 0.072(3) Uani 1 d . . H60A H -0.2818(4) -0.0631(5) -0.0803(4) 0.087 Uiso 1 calc R . C61 C -0.1332(5) 0.1445(5) 0.0583(5) 0.077(3) Uani 1 d . . C62 C -0.1138(5) 0.2014(5) 0.1048(5) 0.077(3) Uani 1 d . . H62A H -0.1416(5) 0.2398(5) 0.1008(5) 0.093 Uiso 1 calc R . C63 C -0.0540(5) 0.2026(5) 0.1573(5) 0.081(3) Uani 1 d . . H63A H -0.0412(5) 0.2426(5) 0.1878(5) 0.097 Uiso 1 calc R . C64 C -0.0113(4) 0.1450(5) 0.1665(4) 0.061(3) Uani 1 d . . C65 C -0.0319(4) 0.0886(5) 0.1184(4) 0.078(3) Uani 1 d . . H65A H -0.0045(4) 0.0501(5) 0.1213(4) 0.093 Uiso 1 calc R . C66 C -0.0939(5) 0.0882(5) 0.0650(5) 0.079(3) Uani 1 d . . H66A H -0.1078(5) 0.0486(5) 0.0341(5) 0.095 Uiso 1 calc R . C67 C 0.0595(4) 0.1362(5) 0.2845(5) 0.078(3) Uani 1 d . . H67A H 0.0244(4) 0.1300(5) 0.2966(5) 0.094 Uiso 1 calc R . C68 C 0.1243(5) 0.1357(4) 0.3412(4) 0.067(3) Uani 1 d . . C69 C 0.1355(5) 0.1193(6) 0.4120(5) 0.100(4) Uani 1 d . . H69A H 0.1019(5) 0.1081(6) 0.4255(5) 0.120 Uiso 1 calc R . C70 C 0.1951(5) 0.1196(7) 0.4605(6) 0.113(5) Uani 1 d . . H70A H 0.2032(5) 0.1074(7) 0.5080(6) 0.135 Uiso 1 calc R . C71 C 0.2441(6) 0.1375(6) 0.4418(5) 0.108(5) Uani 1 d . . H71A H 0.2857(6) 0.1395(6) 0.4759(5) 0.130 Uiso 1 calc R . C72 C 0.2299(5) 0.1528(6) 0.3695(6) 0.099(4) Uani 1 d . . H72A H 0.2632(5) 0.1631(6) 0.3553(6) 0.119 Uiso 1 calc R . B1 B -0.2545(2) -0.4342(3) -0.0129(2) 0.141(5) Uani 1 d DU . F11 F -0.2711(3) -0.4632(4) 0.0393(3) 0.160(3) Uani 1 d DU . F12 F -0.2392(14) -0.3706(6) 0.0241(9) 0.173(9) Uani 0.331(8) d PDU 1 F13 F -0.2737(12) -0.4474(15) -0.0847(5) 0.173(9) Uani 0.331(8) d PDU 1 F14 F -0.2026(5) -0.4783(8) 0.0123(13) 0.171(9) Uani 0.331(8) d PDU 1 F12' F -0.2589(7) -0.3605(4) -0.0152(7) 0.163(5) Uani 0.669(8) d PDU 2 F13' F -0.2988(5) -0.4544(8) -0.0783(4) 0.151(5) Uani 0.669(8) d PDU 2 F14' F -0.1923(3) -0.4439(8) -0.0020(6) 0.161(5) Uani 0.669(8) d PDU 2 B2 B -0.2986(3) -0.1027(3) 0.0913(3) 0.161(6) Uani 1 d DU . F21 F -0.3077(5) -0.1751(3) 0.0801(4) 0.169(4) Uani 1 d DU . F22 F -0.3562(4) -0.0690(8) 0.0672(11) 0.184(7) Uani 0.474(7) d PDU 1 F23 F -0.2638(8) -0.0883(9) 0.1614(5) 0.161(6) Uani 0.474(7) d PDU 1 F24 F -0.2641(5) -0.0884(10) 0.0516(6) 0.171(6) Uani 0.474(7) d PDU 1 F22' F -0.3071(6) -0.0870(8) 0.1524(5) 0.146(5) Uani 0.526(7) d PDU 2 F23' F -0.2379(4) -0.0773(9) 0.1142(10) 0.192(7) Uani 0.526(7) d PDU 2 F24' F -0.3244(9) -0.0639(7) 0.0301(5) 0.180(7) Uani 0.526(7) d PDU 2 B3 B 0.0398(2) -0.2882(3) -0.1088(3) 0.142(5) Uani 1 d DU . F31 F 0.1042(2) -0.2870(5) -0.0879(3) 0.151(3) Uani 1 d DU . F32 F 0.0096(5) -0.3315(7) -0.0777(6) 0.154(6) Uani 0.514(7) d PDU 1 F33 F 0.0148(6) -0.2295(6) -0.0882(8) 0.177(7) Uani 0.514(7) d PDU 1 F34 F 0.0063(6) -0.2965(7) -0.1810(4) 0.120(5) Uani 0.514(7) d PDU 1 F32' F 0.0411(8) -0.3599(4) -0.0917(8) 0.145(6) Uani 0.486(7) d PDU 2 F33' F 0.0440(9) -0.2388(7) -0.0569(7) 0.197(8) Uani 0.486(7) d PDU 2 F34' F 0.0163(9) -0.2597(8) -0.1764(5) 0.147(6) Uani 0.486(7) d PDU 2 B4 B 0.4041(2) 0.1521(3) 0.4216(3) 0.145(5) Uani 1 d DU . F41 F 0.4229(7) 0.1373(7) 0.4933(4) 0.204(6) Uani 0.717(6) d PDU 1 F42 F 0.3718(5) 0.2162(4) 0.3998(7) 0.156(5) Uani 0.717(6) d PDU 1 F43 F 0.3693(5) 0.0958(4) 0.3814(6) 0.157(5) Uani 0.717(6) d PDU 1 F44 F 0.4638(3) 0.1550(7) 0.4213(7) 0.179(5) Uani 0.717(6) d PDU 1 F41' F 0.4641(5) 0.1248(12) 0.4557(17) 0.169(9) Uani 0.283(6) d PDU 2 F42' F 0.3594(6) 0.0993(8) 0.4098(17) 0.143(9) Uani 0.283(6) d PDU 2 F43' F 0.4183(8) 0.1811(13) 0.3674(7) 0.182(10) Uani 0.283(6) d PDU 2 F44' F 0.3908(7) 0.1721(15) 0.4792(7) 0.169(9) Uani 0.283(6) d PDU 2 N13 N 0.2901(9) -0.1138(11) 0.1389(9) 0.142(7) Uani 0.611(7) d PU 1 C73 C 0.3878(11) -0.0789(13) 0.1344(13) 0.153(9) Uani 0.611(7) d PU 1 H73A H 0.3991(11) -0.1048(13) 0.0998(13) 0.229 Uiso 0.611(7) d PR 1 H73B H 0.3846(11) -0.0279(13) 0.1233(13) 0.229 Uiso 0.611(7) d PR 1 H73C H 0.4199(11) -0.0865(13) 0.1818(13) 0.229 Uiso 0.611(7) d PR 1 C74 C 0.3344(11) -0.1013(13) 0.1348(11) 0.124(8) Uani 0.611(7) d PU 1 N13' N 0.0358(14) -0.4186(10) 0.1294(15) 0.148(11) Uani 0.389(7) d PU 2 C73' C -0.0389(14) -0.4539(16) 0.0098(16) 0.133(12) Uani 0.389(7) d PU 2 H73D H -0.0749(14) -0.4817(16) 0.0089(16) 0.200 Uiso 0.389(7) d PR 2 H73E H -0.0535(14) -0.4094(16) -0.0164(16) 0.200 Uiso 0.389(7) d PR 2 H73F H -0.0155(14) -0.4815(16) -0.0123(16) 0.200 Uiso 0.389(7) d PR 2 C74' C -0.0042(16) -0.4384(14) 0.0730(21) 0.140(11) Uani 0.389(7) d PU 2 O4 O -0.0126(17) -0.5243(19) -0.1817(21) 0.159(6) Uani 0.263(7) d PU 1 C75 C -0.0430(30) -0.5433(31) -0.2099(34) 0.157(8) Uani 0.263(7) d PU 1 O4' O 0.0600(19) -0.5171(21) -0.1042(23) 0.158(6) Uani 0.237(7) d PU 2 C75' C 0.0347(32) -0.5175(36) -0.0604(36) 0.162(8) Uani 0.237(7) d PU 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0742(7) 0.0659(6) 0.0533(5) -0.0077(6) 0.0177(5) -0.0024(7) Co2 0.0611(7) 0.0790(7) 0.0680(6) 0.0062(6) 0.0177(6) -0.0075(7) O1 0.105(5) 0.063(4) 0.088(4) 0.011(3) -0.001(4) 0.002(4) O2 0.146(5) 0.093(4) 0.067(3) -0.007(3) 0.052(3) -0.035(4) O3 0.070(4) 0.068(3) 0.078(3) -0.031(3) -0.005(3) 0.007(3) N1 0.081(5) 0.064(4) 0.063(4) -0.018(4) 0.011(4) -0.012(4) N2 0.094(5) 0.063(4) 0.054(3) 0.002(3) 0.038(3) -0.009(4) N3 0.056(4) 0.082(5) 0.060(4) 0.010(3) 0.024(3) 0.019(4) N4 0.070(4) 0.120(7) 0.089(5) 0.018(5) 0.039(4) -0.007(5) N5 0.083(5) 0.063(4) 0.068(4) -0.012(4) 0.026(4) -0.003(4) N6 0.078(4) 0.060(4) 0.054(3) -0.007(3) 0.017(3) 0.014(4) N7 0.065(4) 0.056(4) 0.075(4) -0.011(3) 0.016(4) 0.001(4) N8 0.087(5) 0.076(5) 0.059(4) 0.004(4) 0.025(4) -0.011(4) N9 0.089(5) 0.082(5) 0.059(4) -0.021(4) 0.015(4) -0.015(5) N10 0.077(5) 0.068(5) 0.080(5) 0.000(4) 0.030(4) 0.010(4) N11 0.048(4) 0.058(4) 0.056(3) -0.003(3) 0.011(3) 0.001(4) N12 0.052(4) 0.086(5) 0.067(4) 0.000(4) 0.023(3) -0.007(4) C1 0.078(6) 0.112(8) 0.062(5) -0.020(5) 0.008(5) -0.013(6) C2 0.071(6) 0.105(8) 0.109(7) -0.024(6) 0.035(6) -0.008(6) C3 0.087(6) 0.092(7) 0.115(7) -0.019(6) 0.045(6) -0.037(6) C4 0.108(7) 0.083(7) 0.082(5) 0.001(5) 0.048(5) -0.020(6) C5 0.088(6) 0.058(5) 0.077(6) -0.008(5) 0.031(5) -0.010(5) C6 0.116(7) 0.041(5) 0.062(5) 0.000(4) 0.037(5) 0.014(5) C7 0.099(6) 0.061(5) 0.030(4) 0.001(4) 0.011(4) -0.021(5) C8 0.135(9) 0.073(6) 0.072(6) -0.006(5) -0.004(6) 0.041(7) C9 0.136(10) 0.086(7) 0.087(7) -0.017(6) -0.001(7) 0.029(7) C10 0.074(6) 0.079(6) 0.065(5) 0.020(5) 0.005(5) 0.015(6) C11 0.107(9) 0.097(8) 0.142(9) -0.050(7) -0.022(8) 0.016(8) C12 0.093(8) 0.071(6) 0.137(9) -0.033(7) 0.002(7) 0.011(6) C13 0.085(6) 0.070(6) 0.065(5) 0.001(5) 0.003(5) 0.028(6) C14 0.145(10) 0.099(7) 0.057(5) -0.014(5) 0.025(6) 0.022(7) C15 0.110(8) 0.068(6) 0.087(6) -0.015(5) 0.026(6) 0.000(6) C16 0.066(5) 0.064(5) 0.059(5) 0.004(4) 0.014(4) -0.005(5) C17 0.092(6) 0.070(6) 0.062(5) 0.005(4) 0.033(5) 0.022(5) C18 0.101(6) 0.058(5) 0.082(5) 0.020(5) 0.042(5) 0.030(5) C19 0.074(6) 0.073(6) 0.094(6) -0.001(5) 0.029(5) 0.009(6) C20 0.089(7) 0.104(8) 0.077(6) 0.002(6) 0.027(5) -0.016(7) C21 0.064(6) 0.185(13) 0.181(10) -0.001(10) 0.066(7) -0.001(8) C22 0.078(7) 0.252(18) 0.207(13) 0.028(12) 0.084(8) -0.015(11) C23 0.108(8) 0.187(13) 0.175(12) -0.025(10) 0.071(8) -0.070(9) C24 0.081(7) 0.121(9) 0.113(8) 0.032(7) 0.019(7) -0.031(7) C25 0.121(7) 0.053(5) 0.079(5) -0.002(5) 0.038(5) -0.008(6) C26 0.150(10) 0.058(6) 0.080(6) -0.011(5) 0.022(7) -0.008(7) C27 0.132(10) 0.066(7) 0.118(8) 0.004(6) 0.017(8) 0.014(8) C28 0.110(8) 0.052(6) 0.216(12) -0.028(7) 0.065(8) 0.004(6) C29 0.060(6) 0.071(6) 0.097(6) -0.014(5) 0.013(5) -0.004(6) C30 0.086(6) 0.076(7) 0.101(6) -0.003(5) 0.049(5) -0.010(6) C31 0.065(5) 0.056(5) 0.070(5) -0.009(4) 0.028(4) -0.014(5) C32 0.089(6) 0.080(6) 0.066(5) -0.001(5) 0.023(5) -0.021(6) C33 0.087(6) 0.111(8) 0.058(5) 0.005(5) 0.031(4) -0.002(6) C34 0.083(5) 0.075(6) 0.060(4) -0.003(4) 0.038(4) -0.025(5) C35 0.144(8) 0.087(7) 0.060(5) 0.004(5) 0.040(5) -0.029(7) C36 0.103(7) 0.079(6) 0.084(6) 0.001(5) 0.027(6) -0.036(6) C37 0.111(7) 0.076(6) 0.074(5) -0.002(5) 0.051(5) -0.025(6) C38 0.103(7) 0.106(7) 0.060(5) -0.002(5) 0.026(5) -0.015(7) C39 0.086(6) 0.073(6) 0.097(6) 0.000(5) 0.052(5) -0.006(5) C40 0.078(5) 0.066(6) 0.097(6) 0.020(5) 0.054(5) 0.009(5) C41 0.101(7) 0.074(6) 0.077(6) -0.014(5) 0.025(5) -0.007(6) C42 0.106(8) 0.080(7) 0.091(7) 0.004(5) 0.032(6) 0.014(6) C43 0.074(6) 0.085(6) 0.075(5) -0.002(5) 0.015(5) 0.000(6) C44 0.069(6) 0.068(6) 0.088(6) -0.014(5) 0.028(5) -0.010(5) C45 0.116(9) 0.105(8) 0.102(7) -0.012(7) 0.029(7) -0.008(8) C46 0.195(12) 0.056(6) 0.124(8) -0.026(6) 0.065(8) -0.031(7) C47 0.128(8) 0.104(8) 0.100(7) -0.021(6) 0.064(6) -0.040(7) C48 0.108(8) 0.087(7) 0.086(6) -0.028(6) 0.024(6) -0.009(7) C49 0.104(7) 0.092(7) 0.060(5) -0.026(5) 0.016(5) -0.010(6) C50 0.204(13) 0.126(9) 0.071(6) -0.039(6) 0.029(8) -0.034(10) C51 0.271(21) 0.204(15) 0.079(8) -0.015(10) -0.012(12) -0.086(15) C52 0.247(15) 0.096(8) 0.038(5) -0.019(5) -0.002(8) -0.026(10) C53 0.125(9) 0.069(6) 0.059(5) -0.015(5) 0.014(6) 0.003(6) C54 0.107(8) 0.074(6) 0.064(5) 0.012(5) 0.018(6) 0.014(6) C55 0.052(5) 0.051(5) 0.067(5) 0.003(4) 0.007(4) 0.002(4) C56 0.063(6) 0.080(6) 0.067(5) -0.012(5) 0.018(5) 0.007(5) C57 0.073(6) 0.073(6) 0.091(6) -0.021(5) 0.037(5) -0.001(5) C58 0.053(5) 0.067(6) 0.065(5) 0.010(5) -0.001(5) 0.020(5) C59 0.066(5) 0.059(5) 0.076(5) -0.001(5) 0.021(5) 0.006(5) C60 0.094(6) 0.050(5) 0.066(5) -0.006(4) 0.023(5) 0.021(5) C61 0.076(6) 0.058(5) 0.076(6) -0.001(5) 0.008(5) 0.004(5) C62 0.087(6) 0.054(5) 0.081(6) -0.017(5) 0.022(5) -0.001(5) C63 0.083(6) 0.073(6) 0.072(5) -0.017(5) 0.014(5) -0.012(6) C64 0.054(5) 0.065(5) 0.059(5) -0.003(4) 0.017(4) 0.000(5) C65 0.069(6) 0.076(6) 0.070(5) -0.005(5) 0.007(5) 0.019(5) C66 0.077(6) 0.064(6) 0.086(6) -0.020(5) 0.020(5) -0.012(5) C67 0.083(6) 0.092(7) 0.071(5) -0.007(5) 0.041(5) -0.011(6) C68 0.075(6) 0.053(5) 0.056(5) -0.009(4) 0.006(5) 0.002(5) C69 0.078(7) 0.130(9) 0.078(6) 0.004(6) 0.015(6) -0.015(7) C70 0.094(8) 0.146(10) 0.072(6) 0.006(7) 0.004(6) 0.030(8) C71 0.079(8) 0.130(9) 0.069(6) -0.022(7) -0.023(6) 0.006(8) C72 0.047(6) 0.140(9) 0.092(7) 0.007(7) 0.005(5) 0.003(6) B1 0.143(8) 0.168(9) 0.155(8) 0.045(8) 0.102(7) 0.007(8) F11 0.218(7) 0.142(6) 0.152(5) 0.014(4) 0.107(5) 0.014(6) F12 0.197(15) 0.164(15) 0.163(14) 0.047(13) 0.074(13) 0.008(14) F13 0.153(14) 0.210(16) 0.172(14) 0.023(14) 0.081(12) 0.027(14) F14 0.139(13) 0.192(16) 0.199(14) 0.070(14) 0.084(12) -0.005(14) F12' 0.197(10) 0.102(6) 0.194(9) 0.068(7) 0.081(8) 0.022(7) F13' 0.137(8) 0.220(10) 0.122(6) 0.032(7) 0.077(5) -0.021(8) F14' 0.121(7) 0.219(11) 0.172(8) 0.071(8) 0.087(6) 0.012(8) B2 0.206(10) 0.126(9) 0.161(9) -0.012(8) 0.083(8) -0.011(9) F21 0.241(8) 0.135(6) 0.129(5) -0.020(5) 0.071(5) -0.014(6) F22 0.205(13) 0.148(11) 0.191(12) 0.006(11) 0.066(11) 0.000(11) F23 0.215(12) 0.126(10) 0.161(10) -0.040(8) 0.093(9) 0.012(10) F24 0.223(11) 0.174(12) 0.158(9) -0.012(9) 0.118(9) -0.025(11) F22' 0.194(11) 0.106(8) 0.174(9) -0.025(8) 0.111(8) -0.003(9) F23' 0.218(12) 0.194(12) 0.185(11) 0.009(11) 0.099(10) -0.001(11) F24' 0.229(13) 0.162(11) 0.137(10) 0.009(9) 0.060(10) -0.043(11) B3 0.118(8) 0.178(10) 0.133(8) 0.022(8) 0.051(7) 0.033(9) F31 0.137(6) 0.195(7) 0.103(4) 0.034(5) 0.027(4) 0.017(6) F32 0.146(9) 0.202(12) 0.134(8) 0.026(9) 0.078(7) -0.045(10) F33 0.108(9) 0.233(13) 0.180(12) 0.011(11) 0.044(9) 0.075(10) F34 0.090(7) 0.141(9) 0.113(8) 0.060(7) 0.022(6) 0.017(8) F32' 0.147(11) 0.143(11) 0.142(10) 0.040(9) 0.055(9) 0.004(10) F33' 0.148(13) 0.241(15) 0.201(14) 0.048(13) 0.067(11) 0.050(13) F34' 0.123(10) 0.185(13) 0.130(9) 0.091(8) 0.046(8) 0.018(10) B4 0.150(8) 0.108(8) 0.211(9) 0.010(8) 0.107(7) -0.033(7) F41 0.203(10) 0.155(9) 0.241(11) 0.039(9) 0.075(9) 0.032(9) F42 0.132(7) 0.085(6) 0.236(9) -0.003(6) 0.055(7) -0.002(6) F43 0.169(8) 0.101(6) 0.216(8) -0.070(6) 0.093(7) -0.030(6) F44 0.163(8) 0.145(8) 0.263(10) 0.002(8) 0.120(7) -0.022(7) F41' 0.178(14) 0.135(14) 0.223(15) 0.042(13) 0.110(13) -0.022(13) F42' 0.138(13) 0.113(14) 0.217(17) -0.030(13) 0.111(13) -0.041(12) F43' 0.160(15) 0.152(15) 0.226(16) 0.006(14) 0.065(14) -0.019(14) F44' 0.150(14) 0.142(15) 0.243(15) 0.008(14) 0.107(12) -0.002(13) N13 0.136(13) 0.170(14) 0.103(10) 0.000(11) 0.028(10) -0.039(12) C73 0.127(15) 0.143(16) 0.181(17) -0.034(14) 0.054(14) 0.000(15) C74 0.105(14) 0.131(13) 0.112(12) -0.033(11) 0.015(12) -0.024(13) N13' 0.168(19) 0.026(9) 0.169(19) 0.001(12) -0.024(17) -0.049(12) C73' 0.091(18) 0.102(17) 0.141(20) 0.032(16) -0.027(17) -0.042(16) C74' 0.117(18) 0.047(12) 0.182(20) 0.019(14) -0.023(17) -0.036(14) O4 0.176(9) 0.117(9) 0.214(9) 0.016(9) 0.110(8) 0.032(9) C75 0.172(11) 0.114(11) 0.213(11) 0.017(11) 0.106(11) 0.037(11) O4' 0.175(9) 0.121(9) 0.210(9) 0.024(9) 0.110(9) 0.029(9) C75' 0.174(12) 0.125(11) 0.215(12) 0.019(11) 0.107(11) 0.028(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.098(8) . ? Co1 N2 2.117(6) . ? Co1 N9 2.132(7) . ? Co1 N6 2.137(8) . ? Co1 N5 2.162(7) . ? Co1 N10 2.167(7) . ? Co2 N8 2.118(8) . ? Co2 N12 2.127(7) . ? Co2 N11 2.160(7) . ? Co2 N4 2.165(8) . ? Co2 N7 2.168(6) . ? Co2 N3 2.192(7) . ? O1 C13 1.356(11) . ? O1 C10 1.389(10) . ? O2 C34 1.349(10) . ? O2 C37 1.421(10) . ? O3 C58 1.376(10) . ? O3 C61 1.390(10) . ? N1 C1 1.315(11) . ? N1 C5 1.347(12) . ? N2 C6 1.240(12) . ? N2 C7 1.428(10) . ? N3 C19 1.273(12) . ? N3 C16 1.425(10) . ? N4 C24 1.342(13) . ? N4 C20 1.364(14) . ? N5 C29 1.325(13) . ? N5 C25 1.355(11) . ? N6 C30 1.302(12) . ? N6 C31 1.424(11) . ? N7 C43 1.283(11) . ? N7 C40 1.444(11) . ? N8 C48 1.324(11) . ? N8 C44 1.334(10) . ? N9 C53 1.324(11) . ? N9 C49 1.345(11) . ? N10 C54 1.299(10) . ? N10 C55 1.454(10) . ? N11 C67 1.263(10) . ? N11 C64 1.417(9) . ? N12 C68 1.321(12) . ? N12 C72 1.336(10) . ? C1 C2 1.400(15) . ? C2 C3 1.293(15) . ? C3 C4 1.419(13) . ? C4 C5 1.347(14) . ? C5 C6 1.502(12) . ? C7 C12 1.363(12) . ? C7 C8 1.393(13) . ? C8 C9 1.344(14) . ? C9 C10 1.316(13) . ? C10 C11 1.385(15) . ? C11 C12 1.378(14) . ? C13 C18 1.348(12) . ? C13 C14 1.423(15) . ? C14 C15 1.324(14) . ? C15 C16 1.369(12) . ? C16 C17 1.360(12) . ? C17 C18 1.421(12) . ? C19 C20 1.494(14) . ? C20 C21 1.37(2) . ? C21 C22 1.42(2) . ? C22 C23 1.35(2) . ? C23 C24 1.33(2) . ? C25 C26 1.356(13) . ? C26 C27 1.42(2) . ? C27 C28 1.35(2) . ? C28 C29 1.406(14) . ? C29 C30 1.431(14) . ? C31 C32 1.342(12) . ? C31 C36 1.367(11) . ? C32 C33 1.398(13) . ? C33 C34 1.384(11) . ? C34 C35 1.377(12) . ? C35 C36 1.353(13) . ? C37 C42 1.374(13) . ? C37 C38 1.414(15) . ? C38 C39 1.334(12) . ? C39 C40 1.392(12) . ? C40 C41 1.359(14) . ? C41 C42 1.357(12) . ? C43 C44 1.447(13) . ? C44 C45 1.375(14) . ? C45 C46 1.407(15) . ? C46 C47 1.406(14) . ? C47 C48 1.356(14) . ? C49 C50 1.339(13) . ? C50 C51 1.43(2) . ? C51 C52 1.36(2) . ? C52 C53 1.331(12) . ? C53 C54 1.405(12) . ? C55 C56 1.368(12) . ? C55 C60 1.369(12) . ? C56 C57 1.415(12) . ? C57 C58 1.351(13) . ? C58 C59 1.376(12) . ? C59 C60 1.392(11) . ? C61 C66 1.341(13) . ? C61 C62 1.358(11) . ? C62 C63 1.361(12) . ? C63 C64 1.402(12) . ? C64 C65 1.370(11) . ? C65 C66 1.401(12) . ? C67 C68 1.473(12) . ? C68 C69 1.380(13) . ? C69 C70 1.328(13) . ? C70 C71 1.35(2) . ? C71 C72 1.391(15) . ? B1 F12 1.357(9) . ? B1 F14' 1.358(8) . ? B1 F12' 1.358(7) . ? B1 F14 1.359(9) . ? B1 F11 1.359(6) . ? B1 F13 1.360(9) . ? B1 F13' 1.362(7) . ? B2 F24' 1.346(8) . ? B2 F24 1.348(9) . ? B2 F23 1.350(8) . ? B2 F22' 1.351(9) . ? B2 F21 1.353(6) . ? B2 F23' 1.359(8) . ? B2 F22 1.358(9) . ? B3 F32 1.355(9) . ? B3 F34' 1.358(8) . ? B3 F31 1.359(6) . ? B3 F33 1.359(9) . ? B3 F32' 1.359(8) . ? B3 F34 1.361(7) . ? B3 F33' 1.361(9) . ? B4 F42' 1.360(9) . ? B4 F44' 1.361(10) . ? B4 F43 1.362(8) . ? B4 F43' 1.362(10) . ? B4 F44 1.362(8) . ? B4 F41' 1.363(9) . ? B4 F41 1.365(8) . ? B4 F42 1.369(7) . ? N13 C74 1.07(3) . ? C73 C74 1.29(3) . ? N13' C74' 1.20(4) . ? C73' C74' 1.24(4) . ? O4 C75 0.79(7) . ? O4' C75' 1.23(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N2 78.3(3) . . ? N1 Co1 N9 92.5(3) . . ? N2 Co1 N9 170.9(3) . . ? N1 Co1 N6 176.7(3) . . ? N2 Co1 N6 98.6(3) . . ? N9 Co1 N6 90.5(3) . . ? N1 Co1 N5 102.2(3) . . ? N2 Co1 N5 88.5(3) . . ? N9 Co1 N5 94.1(3) . . ? N6 Co1 N5 76.4(3) . . ? N1 Co1 N10 89.6(3) . . ? N2 Co1 N10 102.8(3) . . ? N9 Co1 N10 76.3(3) . . ? N6 Co1 N10 92.3(3) . . ? N5 Co1 N10 165.2(3) . . ? N8 Co2 N12 91.5(3) . . ? N8 Co2 N11 90.4(3) . . ? N12 Co2 N11 77.2(2) . . ? N8 Co2 N4 93.9(3) . . ? N12 Co2 N4 96.3(3) . . ? N11 Co2 N4 172.3(3) . . ? N8 Co2 N7 77.1(2) . . ? N12 Co2 N7 163.5(3) . . ? N11 Co2 N7 90.8(3) . . ? N4 Co2 N7 96.4(3) . . ? N8 Co2 N3 171.7(3) . . ? N12 Co2 N3 91.7(3) . . ? N11 Co2 N3 97.7(3) . . ? N4 Co2 N3 78.2(3) . . ? N7 Co2 N3 101.2(2) . . ? C13 O1 C10 117.4(7) . . ? C34 O2 C37 114.1(7) . . ? C58 O3 C61 116.9(7) . . ? C1 N1 C5 114.6(9) . . ? C1 N1 Co1 130.2(7) . . ? C5 N1 Co1 115.1(6) . . ? C6 N2 C7 116.8(7) . . ? C6 N2 Co1 113.0(5) . . ? C7 N2 Co1 130.2(6) . . ? C19 N3 C16 119.3(8) . . ? C19 N3 Co2 113.1(6) . . ? C16 N3 Co2 127.5(6) . . ? C24 N4 C20 118.5(10) . . ? C24 N4 Co2 129.6(8) . . ? C20 N4 Co2 111.9(7) . . ? C29 N5 C25 120.1(8) . . ? C29 N5 Co1 113.4(6) . . ? C25 N5 Co1 126.3(7) . . ? C30 N6 C31 117.1(8) . . ? C30 N6 Co1 113.9(6) . . ? C31 N6 Co1 128.9(6) . . ? C43 N7 C40 116.6(7) . . ? C43 N7 Co2 112.5(6) . . ? C40 N7 Co2 130.5(5) . . ? C48 N8 C44 118.7(8) . . ? C48 N8 Co2 126.5(6) . . ? C44 N8 Co2 114.4(6) . . ? C53 N9 C49 119.6(8) . . ? C53 N9 Co1 115.0(6) . . ? C49 N9 Co1 125.0(6) . . ? C54 N10 C55 117.3(7) . . ? C54 N10 Co1 111.6(6) . . ? C55 N10 Co1 131.0(5) . . ? C67 N11 C64 118.2(8) . . ? C67 N11 Co2 112.6(6) . . ? C64 N11 Co2 128.4(5) . . ? C68 N12 C72 117.1(8) . . ? C68 N12 Co2 114.3(5) . . ? C72 N12 Co2 128.6(7) . . ? N1 C1 C2 123.6(9) . . ? C3 C2 C1 122.4(9) . . ? C2 C3 C4 114.6(10) . . ? C5 C4 C3 120.9(10) . . ? N1 C5 C4 123.4(8) . . ? N1 C5 C6 111.8(9) . . ? C4 C5 C6 124.7(9) . . ? N2 C6 C5 121.7(8) . . ? C12 C7 C8 117.6(8) . . ? C12 C7 N2 120.6(8) . . ? C8 C7 N2 121.4(7) . . ? C9 C8 C7 122.2(9) . . ? C10 C9 C8 119.9(10) . . ? C9 C10 C11 120.5(9) . . ? C9 C10 O1 118.1(9) . . ? C11 C10 O1 121.4(8) . . ? C12 C11 C10 120.0(10) . . ? C7 C12 C11 119.6(10) . . ? C18 C13 O1 120.4(10) . . ? C18 C13 C14 119.0(9) . . ? O1 C13 C14 120.5(8) . . ? C15 C14 C13 119.2(9) . . ? C14 C15 C16 123.0(11) . . ? C17 C16 C15 119.2(9) . . ? C17 C16 N3 118.2(7) . . ? C15 C16 N3 122.5(9) . . ? C16 C17 C18 119.3(8) . . ? C13 C18 C17 120.2(9) . . ? N3 C19 C20 119.5(9) . . ? N4 C20 C21 122.1(11) . . ? N4 C20 C19 117.3(10) . . ? C21 C20 C19 120.5(12) . . ? C20 C21 C22 117.6(13) . . ? C23 C22 C21 117.6(13) . . ? C24 C23 C22 122.9(14) . . ? C23 C24 N4 121.0(13) . . ? N5 C25 C26 122.1(12) . . ? C25 C26 C27 117.7(11) . . ? C28 C27 C26 120.4(11) . . ? C27 C28 C29 118.8(12) . . ? N5 C29 C28 120.9(10) . . ? N5 C29 C30 117.0(9) . . ? C28 C29 C30 122.2(10) . . ? N6 C30 C29 118.5(10) . . ? C32 C31 C36 118.8(8) . . ? C32 C31 N6 122.3(7) . . ? C36 C31 N6 118.8(8) . . ? C31 C32 C33 119.6(8) . . ? C34 C33 C32 121.2(8) . . ? O2 C34 C35 125.2(7) . . ? O2 C34 C33 117.3(8) . . ? C35 C34 C33 117.5(9) . . ? C36 C35 C34 119.9(8) . . ? C35 C36 C31 122.8(9) . . ? C42 C37 C38 121.6(9) . . ? C42 C37 O2 119.9(9) . . ? C38 C37 O2 118.4(8) . . ? C39 C38 C37 116.8(9) . . ? C38 C39 C40 122.2(10) . . ? C41 C40 C39 119.7(9) . . ? C41 C40 N7 119.9(8) . . ? C39 C40 N7 120.4(9) . . ? C42 C41 C40 120.4(10) . . ? C41 C42 C37 119.2(11) . . ? N7 C43 C44 119.9(8) . . ? N8 C44 C45 122.7(9) . . ? N8 C44 C43 115.9(8) . . ? C45 C44 C43 121.5(9) . . ? C44 C45 C46 119.8(10) . . ? C47 C46 C45 115.0(10) . . ? C48 C47 C46 121.5(10) . . ? N8 C48 C47 122.2(9) . . ? C50 C49 N9 122.8(10) . . ? C49 C50 C51 115.7(11) . . ? C52 C51 C50 120.7(12) . . ? C53 C52 C51 118.6(11) . . ? N9 C53 C52 122.5(9) . . ? N9 C53 C54 115.5(8) . . ? C52 C53 C54 122.0(9) . . ? N10 C54 C53 121.5(9) . . ? C56 C55 C60 121.1(8) . . ? C56 C55 N10 119.1(8) . . ? C60 C55 N10 119.6(8) . . ? C55 C56 C57 118.9(9) . . ? C58 C57 C56 120.2(9) . . ? C57 C58 C59 120.2(8) . . ? C57 C58 O3 120.3(8) . . ? C59 C58 O3 119.5(9) . . ? C58 C59 C60 120.3(9) . . ? C55 C60 C59 119.2(9) . . ? C66 C61 C62 120.0(8) . . ? C66 C61 O3 123.0(8) . . ? C62 C61 O3 117.0(8) . . ? C61 C62 C63 120.4(9) . . ? C62 C63 C64 121.6(8) . . ? C65 C64 C63 116.7(7) . . ? C65 C64 N11 120.0(8) . . ? C63 C64 N11 123.2(7) . . ? C64 C65 C66 120.8(9) . . ? C61 C66 C65 120.4(8) . . ? N11 C67 C68 119.9(9) . . ? N12 C68 C69 122.8(8) . . ? N12 C68 C67 115.3(8) . . ? C69 C68 C67 121.9(10) . . ? C70 C69 C68 118.9(11) . . ? C69 C70 C71 121.0(11) . . ? C70 C71 C72 117.4(10) . . ? N12 C72 C71 122.8(11) . . ? F14' B1 F12' 101.2(10) . . ? F12 B1 F14 108.0(14) . . ? F12 B1 F11 90.1(11) . . ? F14' B1 F11 114.3(7) . . ? F12' B1 F11 112.2(8) . . ? F14 B1 F11 86.6(11) . . ? F12 B1 F13 130.1(15) . . ? F14 B1 F13 99.4(16) . . ? F11 B1 F13 133.1(13) . . ? F14' B1 F13' 117.1(8) . . ? F12' B1 F13' 102.8(8) . . ? F11 B1 F13' 108.4(7) . . ? F24 B2 F23 110.0(10) . . ? F24' B2 F22' 123.7(11) . . ? F24' B2 F21 112.7(7) . . ? F24 B2 F21 100.4(10) . . ? F23 B2 F21 110.9(8) . . ? F22' B2 F21 107.2(8) . . ? F24' B2 F23' 98.8(12) . . ? F22' B2 F23' 96.0(10) . . ? F21 B2 F23' 117.7(10) . . ? F24 B2 F22 113.9(11) . . ? F23 B2 F22 112.1(12) . . ? F21 B2 F22 109.0(9) . . ? F32 B3 F31 123.2(7) . . ? F34' B3 F31 105.1(9) . . ? F32 B3 F33 88.7(10) . . ? F31 B3 F33 114.9(7) . . ? F34' B3 F32' 126.2(10) . . ? F31 B3 F32' 91.3(9) . . ? F32 B3 F34 104.7(8) . . ? F31 B3 F34 115.0(8) . . ? F33 B3 F34 106.8(9) . . ? F34' B3 F33' 113.2(10) . . ? F31 B3 F33' 90.3(9) . . ? F32' B3 F33' 117.7(10) . . ? F42' B4 F44' 86.6(17) . . ? F42' B4 F43' 122.4(17) . . ? F44' B4 F43' 141.2(16) . . ? F43 B4 F44 112.3(9) . . ? F42' B4 F41' 111.1(12) . . ? F44' B4 F41' 100.5(16) . . ? F43' B4 F41' 92.6(15) . . ? F43 B4 F41 110.3(9) . . ? F44 B4 F41 96.4(9) . . ? F43 B4 F42 110.3(6) . . ? F44 B4 F42 112.2(8) . . ? F41 B4 F42 114.7(9) . . ? N13 C74 C73 172.8(29) . . ? N13' C74' C73' 169.3(45) . . ? _refine_diff_density_max 0.403 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.057 #### END of this CIF #### ################################################################ data_Ni1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74.50 H59 B4 F16 N13 Ni2 O3.50' _chemical_formula_weight 1657.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'Cc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.723(8) _cell_length_b 18.472(6) _cell_length_c 20.184(9) _cell_angle_alpha 90.00 _cell_angle_beta 112.71(4) _cell_angle_gamma 90.00 _cell_volume 7815(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 4.50 _cell_measurement_theta_max 10.89 _exptl_crystal_description 'plate ' _exptl_crystal_colour 'orange ' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3380 _exptl_absorpt_coefficient_mu 0.576 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 5.09 _diffrn_reflns_number 7408 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.1597 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.04 _reflns_number_total 6952 _reflns_number_gt 2816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 6952 _refine_ls_number_parameters 1197 _refine_ls_number_restraints 183 _refine_ls_R_factor_all 0.1892 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1426 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.07680(6) 1.19105(7) 0.26320(7) 0.0736(4) Uani 1 1 d . . . Ni2 Ni 0.45851(6) 0.82377(8) 0.65148(7) 0.0784(5) Uani 1 1 d . . . N1 N -0.0110(4) 1.2056(4) 0.2730(4) 0.071(3) Uani 1 1 d . . . N2 N 0.1043(4) 1.2009(4) 0.3754(4) 0.063(2) Uani 1 1 d . . . N3 N 0.4873(3) 0.9318(4) 0.6309(4) 0.062(2) Uani 1 1 d . . . N4 N 0.5519(4) 0.8035(6) 0.6516(5) 0.090(3) Uani 1 1 d . . . N5 N 0.0349(4) 1.1811(5) 0.1489(4) 0.085(3) Uani 1 1 d . . . N6 N 0.0569(4) 1.0760(4) 0.2463(4) 0.077(3) Uani 1 1 d . . . N7 N 0.3704(4) 0.8552(4) 0.6633(4) 0.062(3) Uani 1 1 d . . . N8 N 0.4914(4) 0.8474(5) 0.7631(4) 0.068(3) Uani 1 1 d . . . N9 N 0.1075(4) 1.3002(5) 0.2622(4) 0.069(3) Uani 1 1 d . . . N10 N 0.1697(4) 1.1788(5) 0.2616(4) 0.061(2) Uani 1 1 d . . . N11 N 0.4048(4) 0.7851(4) 0.5439(4) 0.069(3) Uani 1 1 d . . . N12 N 0.4408(4) 0.7123(5) 0.6686(4) 0.073(3) Uani 1 1 d . . . C1 C -0.0708(6) 1.2032(7) 0.2194(6) 0.098(4) Uani 1 1 d . . . H1A H -0.0750 1.1992 0.1719 0.118 Uiso 1 1 calc R . . C2 C -0.1242(6) 1.2066(7) 0.2346(7) 0.100(4) Uani 1 1 d . . . H2A H -0.1638 1.2039 0.1967 0.120 Uiso 1 1 calc R . . C3 C -0.1228(6) 1.2134(6) 0.2986(7) 0.105(4) Uani 1 1 d . . . H3A H -0.1599 1.2176 0.3075 0.126 Uiso 1 1 calc R . . C4 C -0.0601(6) 1.2141(6) 0.3562(6) 0.094(4) Uani 1 1 d . . . H4A H -0.0550 1.2154 0.4041 0.113 Uiso 1 1 calc R . . C5 C -0.0094(5) 1.2127(6) 0.3367(6) 0.073(3) Uani 1 1 d . . . C6 C 0.0580(5) 1.2116(5) 0.3946(5) 0.070(3) Uani 1 1 d . . . H6A H 0.0650 1.2186 0.4427 0.084 Uiso 1 1 calc R . . C7 C 0.1657(5) 1.1987(5) 0.4333(4) 0.070(3) Uani 1 1 d . . . C8 C 0.2118(6) 1.2524(6) 0.4403(6) 0.100(5) Uani 1 1 d . . . H8A H 0.2021 1.2909 0.4082 0.120 Uiso 1 1 calc R . . C9 C 0.2715(7) 1.2477(6) 0.4947(6) 0.116(6) Uani 1 1 d . . . H9A H 0.2994 1.2867 0.5033 0.139 Uiso 1 1 calc R . . C10 C 0.2895(5) 1.1899(6) 0.5342(5) 0.080(4) Uani 1 1 d . . . C11 C 0.2449(6) 1.1348(7) 0.5296(8) 0.132(6) Uani 1 1 d . . . H11A H 0.2563 1.0959 0.5613 0.159 Uiso 1 1 calc R . . C12 C 0.1835(6) 1.1399(6) 0.4763(7) 0.122(6) Uani 1 1 d . . . H12A H 0.1546 1.1024 0.4704 0.147 Uiso 1 1 calc R . . C13 C 0.3827(5) 1.1260(6) 0.5984(6) 0.083(4) Uani 1 1 d . . . C14 C 0.3989(5) 1.0894(5) 0.6599(6) 0.078(4) Uani 1 1 d . . . H14A H 0.3871 1.1070 0.6962 0.094 Uiso 1 1 calc R . . C15 C 0.4342(5) 1.0239(6) 0.6705(5) 0.071(3) Uani 1 1 d . . . H15A H 0.4460 0.9993 0.7139 0.085 Uiso 1 1 calc R . . C16 C 0.4503(5) 0.9977(5) 0.6177(5) 0.060(3) Uani 1 1 d . . . C17 C 0.4334(6) 1.0360(6) 0.5547(6) 0.091(4) Uani 1 1 d . . . H17A H 0.4465 1.0193 0.5190 0.109 Uiso 1 1 calc R . . C18 C 0.3981(6) 1.0978(7) 0.5429(6) 0.101(5) Uani 1 1 d . . . H18A H 0.3845 1.1210 0.4986 0.121 Uiso 1 1 calc R . . C19 C 0.5391(5) 0.9331(6) 0.6227(5) 0.079(4) Uani 1 1 d . . . H19A H 0.5525 0.9760 0.6088 0.094 Uiso 1 1 calc R . . C20 C 0.5800(6) 0.8667(7) 0.6347(6) 0.092(4) Uani 1 1 d . . . C21 C 0.6360(6) 0.8627(11) 0.6286(8) 0.143(7) Uani 1 1 d . . . H21A H 0.6547 0.9039 0.6185 0.172 Uiso 1 1 calc R . . C22 C 0.6675(6) 0.7933(11) 0.6378(9) 0.164(8) Uani 1 1 d . . . H22A H 0.7056 0.7874 0.6312 0.197 Uiso 1 1 calc R . . C23 C 0.6382(8) 0.7363(10) 0.6568(8) 0.155(7) Uani 1 1 d . . . H23A H 0.6590 0.6919 0.6674 0.186 Uiso 1 1 calc R . . C24 C 0.5834(5) 0.7423(8) 0.6603(6) 0.102(5) Uani 1 1 d . . . H24A H 0.5648 0.7007 0.6696 0.123 Uiso 1 1 calc R . . C25 C 0.0265(5) 1.2352(7) 0.1026(5) 0.094(4) Uani 1 1 d . . . H25A H 0.0359 1.2821 0.1203 0.113 Uiso 1 1 calc R . . C26 C 0.0047(8) 1.2247(9) 0.0298(7) 0.146(7) Uani 1 1 d . . . H26A H 0.0006 1.2625 -0.0022 0.175 Uiso 1 1 calc R . . C27 C -0.0113(9) 1.1517(11) 0.0065(8) 0.191(10) Uani 1 1 d . . . H27A H -0.0268 1.1408 -0.0423 0.230 Uiso 1 1 calc R . . C28 C -0.0043(8) 1.0986(7) 0.0543(6) 0.141(7) Uani 1 1 d . . . H28A H -0.0162 1.0515 0.0386 0.169 Uiso 1 1 calc R . . C29 C 0.0198(7) 1.1136(6) 0.1247(6) 0.106(5) Uani 1 1 d . . . C30 C 0.0335(5) 1.0610(6) 0.1775(5) 0.079(4) Uani 1 1 d . . . H30A H 0.0257 1.0128 0.1635 0.095 Uiso 1 1 calc R . . C31 C 0.0719(4) 1.0152(6) 0.2960(5) 0.064(3) Uani 1 1 d . . . C32 C 0.0573(5) 1.0218(5) 0.3561(5) 0.073(4) Uani 1 1 d . . . H32A H 0.0372 1.0632 0.3632 0.088 Uiso 1 1 calc R . . C33 C 0.0733(5) 0.9653(6) 0.4062(5) 0.072(3) Uani 1 1 d . . . H33A H 0.0612 0.9673 0.4453 0.087 Uiso 1 1 calc R . . C34 C 0.1079(5) 0.9051(6) 0.3972(5) 0.067(3) Uani 1 1 d . . . C35 C 0.1206(5) 0.8987(6) 0.3387(6) 0.077(4) Uani 1 1 d . . . H35A H 0.1403 0.8570 0.3314 0.092 Uiso 1 1 calc R . . C36 C 0.1044(4) 0.9558(6) 0.2863(5) 0.063(3) Uani 1 1 d . . . H36A H 0.1156 0.9528 0.2467 0.076 Uiso 1 1 calc R . . C37 C 0.1869(5) 0.8548(6) 0.5040(5) 0.079(4) Uani 1 1 d . . . C38 C 0.2055(5) 0.7988(5) 0.5495(5) 0.071(3) Uani 1 1 d . . . H38A H 0.1772 0.7608 0.5448 0.085 Uiso 1 1 calc R . . C39 C 0.2647(5) 0.7962(6) 0.6021(5) 0.076(4) Uani 1 1 d . . . H39A H 0.2772 0.7566 0.6329 0.091 Uiso 1 1 calc R . . C40 C 0.3079(4) 0.8554(6) 0.6098(5) 0.066(3) Uani 1 1 d . . . C41 C 0.2880(5) 0.9115(6) 0.5618(5) 0.078(4) Uani 1 1 d . . . H41A H 0.3158 0.9496 0.5652 0.093 Uiso 1 1 calc R . . C42 C 0.2280(5) 0.9127(6) 0.5088(6) 0.079(4) Uani 1 1 d . . . H42A H 0.2148 0.9511 0.4767 0.095 Uiso 1 1 calc R . . C43 C 0.3782(5) 0.8631(6) 0.7262(6) 0.074(3) Uani 1 1 d . . . H43A H 0.3425 0.8682 0.7377 0.089 Uiso 1 1 calc R . . C44 C 0.4439(5) 0.8650(5) 0.7864(5) 0.066(3) Uani 1 1 d . . . C45 C 0.4542(6) 0.8811(7) 0.8553(6) 0.098(4) Uani 1 1 d . . . H45A H 0.4205 0.8929 0.8686 0.118 Uiso 1 1 calc R . . C46 C 0.5147(6) 0.8797(8) 0.9041(7) 0.113(5) Uani 1 1 d . . . H46A H 0.5227 0.8903 0.9519 0.135 Uiso 1 1 calc R . . C47 C 0.5649(7) 0.8629(8) 0.8849(6) 0.111(5) Uani 1 1 d . . . H47A H 0.6068 0.8620 0.9183 0.133 Uiso 1 1 calc R . . C48 C 0.5498(5) 0.8473(7) 0.8135(7) 0.100(5) Uani 1 1 d . . . H48A H 0.5833 0.8359 0.7995 0.120 Uiso 1 1 calc R . . C49 C 0.0752(6) 1.3632(6) 0.2691(6) 0.088(4) Uani 1 1 d . . . H49A H 0.0357 1.3591 0.2726 0.105 Uiso 1 1 calc R . . C50 C 0.1012(7) 1.4304(6) 0.2708(6) 0.107(6) Uani 1 1 d . . . H50A H 0.0805 1.4713 0.2778 0.128 Uiso 1 1 calc R . . C51 C 0.1592(7) 1.4375(7) 0.2620(7) 0.117(6) Uani 1 1 d . . . H51A H 0.1755 1.4831 0.2595 0.141 Uiso 1 1 calc R . . C52 C 0.1920(6) 1.3759(6) 0.2571(9) 0.129(6) Uani 1 1 d . . . H52A H 0.2314 1.3781 0.2532 0.155 Uiso 1 1 calc R . . C53 C 0.1617(5) 1.3094(6) 0.2585(6) 0.082(4) Uani 1 1 d . . . C54 C 0.1956(5) 1.2409(6) 0.2531(6) 0.080(4) Uani 1 1 d . . . H54A H 0.2328 1.2420 0.2442 0.096 Uiso 1 1 calc R . . C55 C 0.2065(5) 1.1159(5) 0.2656(5) 0.058(3) Uani 1 1 d . . . C56 C 0.2449(5) 1.0892(6) 0.3306(6) 0.084(4) Uani 1 1 d . . . H56A H 0.2465 1.1127 0.3720 0.101 Uiso 1 1 calc R . . C57 C 0.2816(6) 1.0284(6) 0.3371(5) 0.086(4) Uani 1 1 d . . . H57A H 0.3093 1.0129 0.3822 0.103 Uiso 1 1 calc R . . C58 C 0.2773(4) 0.9913(6) 0.2781(5) 0.061(3) Uani 1 1 d . . . C59 C 0.2370(5) 1.0140(7) 0.2127(6) 0.083(4) Uani 1 1 d . . . H59A H 0.2325 0.9870 0.1721 0.099 Uiso 1 1 calc R . . C60 C 0.2016(5) 1.0781(6) 0.2054(5) 0.078(4) Uani 1 1 d . . . H60A H 0.1751 1.0946 0.1602 0.093 Uiso 1 1 calc R . . C61 C 0.3360(6) 0.8941(6) 0.3473(6) 0.082(4) Uani 1 1 d . . . C62 C 0.2943(6) 0.8503(7) 0.3658(6) 0.096(4) Uani 1 1 d . . . H62A H 0.2520 0.8444 0.3346 0.115 Uiso 1 1 calc R . . C63 C 0.3173(5) 0.8173(6) 0.4298(6) 0.076(3) Uani 1 1 d . . . H63A H 0.2896 0.7902 0.4439 0.091 Uiso 1 1 calc R . . C64 C 0.3802(5) 0.8222(6) 0.4752(6) 0.070(3) Uani 1 1 d . . . C65 C 0.4206(6) 0.8633(6) 0.4552(6) 0.089(4) Uani 1 1 d . . . H65A H 0.4634 0.8669 0.4856 0.107 Uiso 1 1 calc R . . C66 C 0.3991(6) 0.8993(7) 0.3909(6) 0.092(4) Uani 1 1 d . . . H66A H 0.4268 0.9267 0.3772 0.110 Uiso 1 1 calc R . . C67 C 0.3860(5) 0.7194(6) 0.5425(5) 0.075(3) Uani 1 1 d . . . H67A H 0.3612 0.6976 0.4991 0.090 Uiso 1 1 calc R . . O1 O 0.3491(4) 1.1890(4) 0.5885(4) 0.094(3) Uani 1 1 d . . . O2 O 0.1257(3) 0.8517(4) 0.4484(4) 0.081(2) Uani 1 1 d . . . O3 O 0.3124(4) 0.9308(4) 0.2791(4) 0.100(3) Uani 1 1 d . . . C68 C 0.4042(5) 0.6791(6) 0.6100(6) 0.073(3) Uani 1 1 d . . . C69 C 0.3828(6) 0.6074(7) 0.6096(7) 0.107(5) Uani 1 1 d . . . H69A H 0.3562 0.5854 0.5672 0.129 Uiso 1 1 calc R . . C70 C 0.4025(7) 0.5706(7) 0.6745(7) 0.126(6) Uani 1 1 d . . . H70A H 0.3925 0.5221 0.6769 0.152 Uiso 1 1 calc R . . C71 C 0.4375(6) 0.6096(7) 0.7350(7) 0.102(4) Uani 1 1 d . . . H71A H 0.4471 0.5886 0.7799 0.122 Uiso 1 1 calc R . . C72 C 0.4591(6) 0.6795(7) 0.7314(7) 0.100(4) Uani 1 1 d . . . H72A H 0.4861 0.7028 0.7728 0.120 Uiso 1 1 calc R . . B1 B 0.8589(3) 0.7866(4) 1.3352(4) 0.133(8) Uani 1 1 d D . . F11 F 0.9233(3) 0.7876(5) 1.3566(4) 0.157(4) Uani 1 1 d D A . F12 F 0.8284(5) 0.7928(7) 1.2628(4) 0.131(4) Uani 0.728(7) 1 d PDU A 1 F13 F 0.8516(6) 0.7261(6) 1.3696(8) 0.197(6) Uani 0.728(7) 1 d PDU A 1 F14 F 0.8224(8) 0.8155(14) 1.3679(10) 0.126(9) Uani 0.272(7) 1 d PDU A 1 F12' F 0.8526(7) 0.8554(5) 1.3549(7) 0.169(6) Uani 0.728(7) 1 d PDU A 2 F13' F 0.8398(17) 0.7495(11) 1.2724(8) 0.132(11) Uani 0.272(7) 1 d PDU A 2 F14' F 0.8246(9) 0.7602(19) 1.3717(12) 0.159(11) Uani 0.272(7) 1 d PDU A 2 B2 B 0.5645(3) -0.0649(4) 0.4301(4) 0.139(7) Uani 1 1 d D . . F21 F 0.5488(4) -0.0368(5) 0.4837(4) 0.159(3) Uani 1 1 d D B . F22 F 0.5734(13) -0.1310(7) 0.4615(11) 0.174(10) Uani 0.450(12) 1 d PDU B 1 F23 F 0.5186(8) -0.0493(14) 0.3645(6) 0.141(8) Uani 0.450(12) 1 d PDU B 1 F24 F 0.6175(6) -0.0244(11) 0.4421(13) 0.157(10) Uani 0.450(12) 1 d PDU B 1 F22' F 0.5607(11) -0.1381(5) 0.4241(11) 0.167(8) Uani 0.550(12) 1 d PDU B 2 F23' F 0.5360(12) -0.0412(14) 0.3610(7) 0.203(10) Uani 0.550(12) 1 d PDU B 2 F24' F 0.6283(4) -0.0614(13) 0.4461(12) 0.160(8) Uani 0.550(12) 1 d PDU B 2 B3 B 0.7234(3) 0.1524(4) 0.3655(4) 0.120(6) Uani 1 1 d D . . F31 F 0.6915(7) 0.0972(6) 0.3222(8) 0.160(6) Uani 0.650(8) 1 d PDU C 1 F32 F 0.7008(10) 0.2156(6) 0.3298(10) 0.222(10) Uani 0.650(8) 1 d PDU C 1 F33 F 0.7289(7) 0.1429(11) 0.4347(5) 0.198(7) Uani 0.650(8) 1 d PDU C 1 F34 F 0.7857(4) 0.1505(9) 0.3741(8) 0.169(6) Uani 0.650(8) 1 d PDU C 1 F31' F 0.6821(6) 0.0956(7) 0.3503(11) 0.129(10) Uani 0.350(8) 1 d PDU C 2 F32' F 0.7684(8) 0.1442(13) 0.4326(6) 0.217(14) Uani 0.350(8) 1 d PDU C 2 F33' F 0.7514(6) 0.1543(14) 0.3170(7) 0.190(12) Uani 0.350(8) 1 d PDU C 2 F34' F 0.6898(7) 0.2146(6) 0.3604(12) 0.122(8) Uani 0.350(8) 1 d PDU C 2 B4 B 0.5223(3) 0.6016(4) 0.5349(4) 0.137(8) Uani 1 1 d D . . F41 F 0.5131(5) 0.6735(4) 0.5235(5) 0.170(4) Uani 1 1 d D D . F42 F 0.4637(5) 0.5705(11) 0.5121(12) 0.158(9) Uani 0.441(8) 1 d PDU D 1 F43 F 0.5621(11) 0.5837(13) 0.6021(7) 0.170(9) Uani 0.441(8) 1 d PDU D 1 F44 F 0.5566(7) 0.5888(14) 0.4945(8) 0.176(8) Uani 0.441(8) 1 d PDU D 1 F42' F 0.5167(8) 0.5882(9) 0.5980(6) 0.138(6) Uani 0.559(8) 1 d PDU D 2 F43' F 0.5832(5) 0.5775(12) 0.5557(10) 0.199(8) Uani 0.559(8) 1 d PDU D 2 F44' F 0.4953(11) 0.5620(9) 0.4749(7) 0.181(8) Uani 0.559(8) 1 d PDU D 2 N13 N 0.6123(9) 0.1139(12) 0.5834(9) 0.132(7) Uani 0.632(8) 1 d PU E 1 C73 C 0.6552(12) 0.0991(15) 0.5800(13) 0.127(7) Uani 0.632(8) 1 d PU E 1 C74 C 0.7088(12) 0.0784(14) 0.5777(14) 0.147(9) Uani 0.632(8) 1 d PU E 1 H74A H 0.7213 0.1040 0.5438 0.220 Uiso 0.632(8) 1 d PR E 1 H74B H 0.7403 0.0856 0.6253 0.220 Uiso 0.632(8) 1 d PR E 1 H74C H 0.7053 0.0277 0.5664 0.220 Uiso 0.632(8) 1 d PR E 1 N14 N 0.8574(15) -0.0811(11) 0.5737(15) 0.111(9) Uani 0.368(8) 1 d PU E 2 C75 C 0.8199(18) -0.0620(16) 0.520(2) 0.112(9) Uani 0.368(8) 1 d PU E 2 C76 C 0.7810(16) -0.0485(16) 0.4583(17) 0.103(10) Uani 0.368(8) 1 d PU E 2 H76A H 0.7577 -0.0047 0.4564 0.154 Uiso 0.368(8) 1 d PR E 2 H76B H 0.7520 -0.0888 0.4457 0.154 Uiso 0.368(8) 1 d PR E 2 H76C H 0.8018 -0.0454 0.4251 0.154 Uiso 0.368(8) 1 d PR E 2 O4 O 0.8821(13) -0.019(2) 0.8402(17) 0.148(8) Uani 0.230(9) 1 d PDU F 1 C77 C 0.853(2) -0.015(4) 0.893(2) 0.156(13) Uani 0.230(9) 1 d PDU F 1 O4' O 0.8201(14) -0.0220(19) 0.7827(16) 0.149(8) Uani 0.270(9) 1 d PDU F 2 C77' C 0.7681(19) -0.041(3) 0.718(2) 0.140(11) Uani 0.270(9) 1 d PDU F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0762(8) 0.0758(9) 0.0593(7) 0.0073(7) 0.0157(6) 0.0025(9) Ni2 0.0639(8) 0.0853(9) 0.0775(9) -0.0078(8) 0.0180(7) 0.0096(9) N1 0.092(6) 0.069(6) 0.046(4) 0.005(4) 0.021(4) 0.014(5) N2 0.086(5) 0.060(5) 0.053(4) -0.006(4) 0.036(4) 0.015(5) N3 0.044(4) 0.089(6) 0.061(4) -0.015(4) 0.028(4) -0.017(5) N4 0.054(5) 0.136(8) 0.081(5) -0.053(6) 0.027(4) 0.025(6) N5 0.087(6) 0.087(6) 0.064(5) 0.028(5) 0.009(5) 0.006(6) N6 0.080(6) 0.065(6) 0.073(6) 0.011(5) 0.017(5) -0.014(5) N7 0.062(5) 0.061(5) 0.045(4) -0.012(4) 0.003(4) 0.000(5) N8 0.049(5) 0.086(6) 0.065(5) -0.002(5) 0.016(4) 0.008(5) N9 0.068(5) 0.080(6) 0.064(5) 0.010(5) 0.030(4) -0.013(5) N10 0.062(5) 0.075(6) 0.050(4) -0.006(4) 0.028(4) -0.022(5) N11 0.068(6) 0.057(5) 0.076(5) 0.015(4) 0.019(4) -0.008(5) N12 0.084(6) 0.077(6) 0.063(5) -0.011(5) 0.035(5) 0.017(5) C1 0.101(9) 0.132(11) 0.056(6) 0.027(7) 0.024(6) 0.009(9) C2 0.088(8) 0.104(10) 0.112(9) 0.028(8) 0.042(7) 0.014(8) C3 0.121(9) 0.089(9) 0.137(9) 0.021(8) 0.084(8) 0.048(8) C4 0.106(8) 0.105(9) 0.074(7) 0.007(6) 0.037(7) 0.039(8) C5 0.077(7) 0.067(7) 0.074(7) 0.008(6) 0.028(6) 0.021(6) C6 0.118(8) 0.035(6) 0.060(6) 0.000(5) 0.038(6) -0.014(6) C7 0.104(8) 0.066(7) 0.027(5) 0.000(5) 0.013(5) 0.036(7) C8 0.119(10) 0.065(7) 0.083(8) 0.011(6) 0.005(7) -0.037(8) C9 0.136(12) 0.071(8) 0.090(9) 0.003(7) -0.011(9) -0.028(8) C10 0.078(7) 0.061(7) 0.074(7) -0.014(6) 0.000(6) -0.023(7) C11 0.097(10) 0.094(9) 0.163(12) 0.050(9) 0.002(10) -0.012(9) C12 0.072(8) 0.072(8) 0.161(12) 0.031(9) -0.024(9) -0.015(8) C13 0.075(7) 0.100(8) 0.055(6) -0.010(6) 0.002(6) -0.048(7) C14 0.100(8) 0.058(7) 0.079(7) -0.014(6) 0.038(6) -0.036(7) C15 0.079(7) 0.074(8) 0.067(6) -0.002(6) 0.037(5) -0.019(7) C16 0.059(7) 0.062(7) 0.049(6) -0.006(5) 0.009(5) -0.005(6) C17 0.096(8) 0.074(8) 0.085(8) 0.006(7) 0.016(7) -0.030(7) C18 0.120(11) 0.095(9) 0.065(7) 0.020(7) 0.011(7) -0.019(9) C19 0.078(8) 0.060(7) 0.082(7) 0.004(6) 0.014(7) -0.005(7) C20 0.088(9) 0.091(9) 0.089(8) -0.008(7) 0.024(7) -0.009(8) C21 0.049(7) 0.235(19) 0.158(12) -0.005(12) 0.053(8) -0.023(11) C22 0.052(7) 0.24(2) 0.210(17) -0.021(15) 0.059(10) 0.010(12) C23 0.137(12) 0.186(16) 0.151(13) 0.021(12) 0.066(11) 0.093(13) C24 0.056(7) 0.129(11) 0.119(9) -0.035(8) 0.032(7) 0.034(8) C25 0.109(9) 0.103(9) 0.056(6) 0.017(7) 0.016(6) 0.016(8) C26 0.212(16) 0.126(11) 0.064(8) 0.040(8) 0.013(9) 0.027(13) C27 0.23(2) 0.199(18) 0.072(10) 0.013(12) -0.028(12) 0.053(17) C28 0.226(16) 0.092(9) 0.046(7) 0.029(7) -0.012(9) 0.024(11) C29 0.159(13) 0.069(8) 0.053(7) 0.022(6) 0.001(8) -0.004(9) C30 0.085(8) 0.073(7) 0.068(7) -0.015(6) 0.015(6) -0.006(7) C31 0.039(6) 0.064(7) 0.076(7) -0.003(6) 0.007(5) -0.002(6) C32 0.089(8) 0.055(6) 0.058(6) 0.000(5) 0.008(6) -0.022(6) C33 0.057(6) 0.067(7) 0.079(7) 0.014(6) 0.011(6) -0.007(6) C34 0.044(6) 0.064(7) 0.064(7) -0.002(6) -0.012(5) -0.024(6) C35 0.071(7) 0.075(7) 0.082(7) 0.022(6) 0.025(6) -0.008(7) C36 0.046(6) 0.079(7) 0.060(6) 0.003(6) 0.015(5) -0.010(6) C37 0.079(7) 0.061(7) 0.072(7) 0.004(6) 0.003(6) 0.002(7) C38 0.074(7) 0.058(7) 0.073(6) 0.007(5) 0.019(6) -0.002(6) C39 0.071(7) 0.073(8) 0.070(6) 0.009(6) 0.011(6) -0.004(7) C40 0.048(6) 0.080(7) 0.064(6) -0.002(6) 0.016(5) 0.012(6) C41 0.064(7) 0.075(7) 0.065(7) 0.003(6) -0.008(6) -0.013(7) C42 0.091(8) 0.053(6) 0.090(8) 0.027(6) 0.030(7) 0.011(7) C43 0.061(6) 0.085(8) 0.083(7) -0.002(6) 0.036(6) 0.011(6) C44 0.071(7) 0.054(6) 0.058(6) 0.009(5) 0.006(6) -0.004(6) C45 0.086(8) 0.137(11) 0.062(7) -0.008(7) 0.017(6) 0.014(9) C46 0.099(10) 0.141(12) 0.072(8) -0.004(8) 0.004(8) -0.023(10) C47 0.096(10) 0.134(11) 0.059(8) 0.007(8) -0.018(8) 0.009(10) C48 0.053(7) 0.134(11) 0.100(9) -0.023(8) 0.013(7) -0.019(8) C49 0.106(9) 0.073(8) 0.071(7) -0.005(7) 0.020(6) 0.009(8) C50 0.172(14) 0.039(6) 0.073(7) 0.004(6) 0.009(9) -0.017(8) C51 0.122(11) 0.077(9) 0.123(11) -0.003(8) 0.014(9) -0.048(9) C52 0.101(9) 0.042(7) 0.248(15) 0.029(9) 0.073(10) -0.005(8) C53 0.063(7) 0.071(8) 0.095(8) 0.011(7) 0.012(6) 0.001(7) C54 0.079(7) 0.079(8) 0.106(8) 0.010(6) 0.061(6) 0.013(7) C55 0.059(6) 0.050(6) 0.071(6) 0.013(5) 0.033(5) 0.012(5) C56 0.079(8) 0.096(9) 0.070(7) 0.000(6) 0.019(6) 0.030(7) C57 0.110(9) 0.079(8) 0.061(6) -0.005(6) 0.024(6) 0.027(8) C58 0.067(6) 0.072(7) 0.046(5) 0.002(5) 0.025(5) 0.026(6) C59 0.088(7) 0.092(9) 0.080(7) -0.009(6) 0.044(6) -0.003(7) C60 0.076(7) 0.085(8) 0.067(7) -0.009(6) 0.023(6) -0.002(7) C61 0.112(8) 0.076(8) 0.072(7) 0.013(6) 0.052(6) 0.039(7) C62 0.099(9) 0.124(10) 0.055(7) 0.003(7) 0.018(7) 0.016(9) C63 0.075(7) 0.077(7) 0.086(7) -0.009(6) 0.042(6) 0.000(7) C64 0.071(6) 0.064(7) 0.092(7) -0.019(6) 0.050(6) -0.021(6) C65 0.111(9) 0.069(7) 0.066(7) 0.004(6) 0.010(7) 0.013(8) C66 0.101(9) 0.093(9) 0.079(8) -0.003(7) 0.033(7) -0.010(8) C67 0.070(7) 0.095(8) 0.059(6) 0.001(6) 0.023(5) -0.001(7) O1 0.093(6) 0.056(5) 0.092(5) -0.007(4) -0.008(5) -0.002(5) O2 0.068(5) 0.067(5) 0.077(5) 0.022(4) -0.006(4) -0.011(4) O3 0.138(7) 0.100(6) 0.070(5) 0.006(4) 0.049(5) 0.036(6) C68 0.069(7) 0.069(7) 0.080(7) 0.004(6) 0.027(6) -0.002(7) C69 0.111(10) 0.115(11) 0.080(8) 0.017(8) 0.019(8) 0.014(10) C70 0.190(15) 0.065(8) 0.119(11) -0.004(8) 0.055(11) 0.041(10) C71 0.119(9) 0.111(10) 0.097(8) 0.027(7) 0.066(7) 0.045(9) C72 0.105(9) 0.090(9) 0.093(9) 0.025(7) 0.024(7) -0.005(8) B1 0.103(13) 0.151(18) 0.146(16) 0.022(14) 0.048(12) -0.018(14) F11 0.139(7) 0.210(9) 0.103(5) -0.037(6) 0.024(5) -0.015(7) F12 0.100(7) 0.161(10) 0.111(7) -0.046(7) 0.020(6) -0.029(8) F13 0.177(10) 0.160(12) 0.316(15) 0.012(11) 0.164(10) 0.036(10) F14 0.168(16) 0.104(18) 0.156(15) 0.030(15) 0.117(13) 0.035(16) F12' 0.207(13) 0.117(9) 0.152(10) -0.028(8) 0.034(9) 0.036(10) F13' 0.117(19) 0.122(19) 0.119(16) -0.112(14) 0.002(15) -0.011(17) F14' 0.167(18) 0.14(2) 0.231(19) -0.002(19) 0.149(15) 0.030(19) B2 0.142(11) 0.106(14) 0.245(17) -0.019(13) 0.160(12) -0.004(12) F21 0.227(8) 0.139(7) 0.158(6) -0.007(5) 0.125(6) -0.006(7) F22 0.211(17) 0.152(16) 0.187(18) -0.027(14) 0.107(15) 0.004(16) F23 0.113(12) 0.235(18) 0.089(10) -0.025(12) 0.054(9) 0.025(14) F24 0.138(15) 0.157(19) 0.174(15) 0.002(14) 0.057(13) -0.014(14) F22' 0.224(16) 0.098(10) 0.204(17) -0.061(10) 0.109(14) -0.005(11) F23' 0.178(17) 0.232(18) 0.169(16) 0.020(15) 0.034(14) -0.047(16) F24' 0.105(11) 0.184(19) 0.206(15) -0.023(14) 0.077(11) -0.001(12) B3 0.133(13) 0.097(12) 0.154(14) -0.026(11) 0.081(12) -0.059(12) F31 0.167(11) 0.096(9) 0.232(13) -0.071(8) 0.093(10) -0.021(9) F32 0.203(16) 0.182(14) 0.222(17) 0.016(13) 0.017(14) -0.043(13) F33 0.142(12) 0.244(16) 0.213(13) 0.014(13) 0.075(11) -0.041(12) F34 0.111(9) 0.200(12) 0.208(13) -0.076(11) 0.074(9) -0.037(10) F31' 0.120(15) 0.084(15) 0.22(2) -0.040(14) 0.103(15) -0.032(13) F32' 0.15(2) 0.21(2) 0.23(2) -0.01(2) 0.017(19) -0.04(2) F33' 0.119(18) 0.24(2) 0.21(2) -0.05(2) 0.064(17) -0.01(2) F34' 0.082(11) 0.079(13) 0.25(2) -0.037(13) 0.110(12) -0.018(11) B4 0.154(18) 0.074(12) 0.182(19) 0.021(13) 0.062(16) -0.003(13) F41 0.217(9) 0.161(8) 0.130(7) 0.007(6) 0.064(6) -0.008(8) F42 0.131(15) 0.168(17) 0.178(17) -0.004(15) 0.064(13) -0.003(14) F43 0.202(18) 0.177(16) 0.134(14) 0.038(13) 0.068(13) -0.009(16) F44 0.199(15) 0.229(18) 0.149(13) -0.009(14) 0.122(11) 0.034(15) F42' 0.206(15) 0.109(10) 0.135(10) 0.030(8) 0.107(10) 0.011(12) F43' 0.207(15) 0.256(17) 0.153(14) -0.013(14) 0.091(12) 0.008(15) F44' 0.204(17) 0.178(14) 0.136(12) -0.025(11) 0.038(12) 0.057(14) N13 0.119(12) 0.173(13) 0.102(10) 0.006(10) 0.039(10) 0.025(12) C73 0.100(12) 0.153(12) 0.118(11) 0.025(10) 0.031(11) 0.028(12) C74 0.112(14) 0.155(15) 0.162(15) 0.024(13) 0.039(13) 0.016(14) N14 0.142(16) 0.017(10) 0.117(15) 0.008(11) -0.014(14) 0.037(12) C75 0.124(15) 0.039(11) 0.123(14) -0.001(12) -0.009(13) 0.025(12) C76 0.109(18) 0.055(14) 0.103(17) -0.002(14) -0.005(15) 0.020(15) O4 0.123(14) 0.126(13) 0.227(14) 0.078(13) 0.103(12) 0.014(13) C77 0.123(19) 0.13(2) 0.24(2) 0.08(2) 0.092(18) 0.008(19) O4' 0.132(14) 0.118(13) 0.238(15) 0.056(13) 0.115(12) 0.029(13) C77' 0.115(18) 0.116(18) 0.24(2) 0.045(19) 0.122(16) 0.043(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.096(9) . ? Ni1 N2 2.111(7) . ? Ni1 N10 2.135(8) . ? Ni1 N9 2.136(8) . ? Ni1 N5 2.137(8) . ? Ni1 N6 2.173(8) . ? Ni2 N8 2.127(8) . ? Ni2 N12 2.151(9) . ? Ni2 N4 2.153(9) . ? Ni2 N11 2.161(8) . ? Ni2 N7 2.184(9) . ? Ni2 N3 2.189(8) . ? N1 C5 1.280(13) . ? N1 C1 1.372(13) . ? N2 C6 1.269(13) . ? N2 C7 1.433(11) . ? N3 C19 1.252(13) . ? N3 C16 1.444(12) . ? N4 C24 1.314(14) . ? N4 C20 1.435(16) . ? N5 C25 1.332(14) . ? N5 C29 1.334(14) . ? N6 C30 1.309(11) . ? N6 C31 1.456(12) . ? N7 C43 1.221(12) . ? N7 C40 1.415(11) . ? N8 C48 1.325(12) . ? N8 C44 1.372(13) . ? N9 C53 1.275(14) . ? N9 C49 1.411(13) . ? N10 C54 1.331(13) . ? N10 C55 1.416(12) . ? N11 C67 1.283(13) . ? N11 C64 1.451(13) . ? N12 C68 1.308(12) . ? N12 C72 1.318(13) . ? C1 C2 1.364(17) . ? C2 C3 1.286(16) . ? C3 C4 1.450(16) . ? C4 C5 1.354(16) . ? C5 C6 1.526(14) . ? C7 C12 1.353(14) . ? C7 C8 1.410(15) . ? C8 C9 1.378(15) . ? C9 C10 1.300(14) . ? C10 O1 1.374(11) . ? C10 C11 1.415(16) . ? C11 C12 1.398(16) . ? C13 C14 1.335(14) . ? C13 O1 1.364(13) . ? C13 C18 1.396(17) . ? C14 C15 1.421(14) . ? C15 C16 1.344(14) . ? C16 C17 1.376(14) . ? C17 C18 1.363(16) . ? C19 C20 1.501(16) . ? C20 C21 1.327(18) . ? C21 C22 1.45(2) . ? C22 C23 1.38(2) . ? C23 C24 1.279(18) . ? C25 C26 1.371(16) . ? C26 C27 1.43(2) . ? C27 C28 1.34(2) . ? C28 C29 1.339(15) . ? C29 C30 1.387(14) . ? C31 C36 1.377(14) . ? C31 C32 1.381(14) . ? C32 C33 1.401(13) . ? C33 C34 1.413(15) . ? C34 C35 1.327(14) . ? C34 O2 1.370(11) . ? C35 C36 1.437(14) . ? C37 C38 1.338(13) . ? C37 C42 1.398(15) . ? C37 O2 1.412(11) . ? C38 C39 1.356(12) . ? C39 C40 1.437(14) . ? C40 C41 1.371(14) . ? C41 C42 1.370(13) . ? C43 C44 1.518(13) . ? C44 C45 1.351(14) . ? C45 C46 1.348(15) . ? C46 C47 1.374(19) . ? C47 C48 1.377(16) . ? C49 C50 1.370(15) . ? C50 C51 1.402(19) . ? C51 C52 1.384(19) . ? C52 C53 1.412(16) . ? C53 C54 1.507(16) . ? C55 C56 1.359(13) . ? C55 C60 1.368(14) . ? C56 C57 1.374(14) . ? C57 C58 1.344(13) . ? C58 C59 1.350(12) . ? C58 O3 1.369(11) . ? C59 C60 1.406(14) . ? C61 C66 1.364(15) . ? C61 C62 1.402(17) . ? C61 O3 1.440(12) . ? C62 C63 1.338(15) . ? C63 C64 1.371(14) . ? C64 C65 1.369(16) . ? C65 C66 1.368(14) . ? C67 C68 1.465(15) . ? C68 C69 1.409(16) . ? C69 C70 1.386(17) . ? C70 C71 1.377(16) . ? C71 C72 1.393(17) . ? B1 F14' 1.354(11) . ? B1 F14 1.354(10) . ? B1 F13' 1.356(10) . ? B1 F11 1.356(8) . ? B1 F12' 1.357(9) . ? B1 F12 1.359(8) . ? B1 F13 1.360(9) . ? F13 F14 1.77(3) . ? B2 F22 1.355(10) . ? B2 F24 1.358(10) . ? B2 F22' 1.358(9) . ? B2 F24' 1.359(9) . ? B2 F23 1.362(9) . ? B2 F23' 1.362(10) . ? B2 F21 1.366(8) . ? B3 F32' 1.354(9) . ? B3 F31 1.356(9) . ? B3 F33' 1.357(9) . ? B3 F34 1.360(9) . ? B3 F31' 1.360(9) . ? B3 F34' 1.362(9) . ? B3 F32 1.364(9) . ? B3 F33 1.366(9) . ? B4 F44' 1.344(9) . ? B4 F43 1.348(10) . ? B4 F44 1.348(10) . ? B4 F41 1.350(8) . ? B4 F42' 1.351(9) . ? B4 F42 1.357(9) . ? B4 F43' 1.357(9) . ? N13 C73 1.04(3) . ? C73 C74 1.30(3) . ? N14 C75 1.14(4) . ? C75 C76 1.25(4) . ? O4 C77 1.44(2) . ? O4' C77' 1.43(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 77.7(3) . . ? N1 Ni1 N10 175.6(3) . . ? N2 Ni1 N10 98.1(3) . . ? N1 Ni1 N9 101.9(3) . . ? N2 Ni1 N9 88.1(3) . . ? N10 Ni1 N9 76.8(3) . . ? N1 Ni1 N5 94.0(3) . . ? N2 Ni1 N5 171.6(4) . . ? N10 Ni1 N5 90.3(3) . . ? N9 Ni1 N5 94.7(3) . . ? N1 Ni1 N6 89.6(3) . . ? N2 Ni1 N6 102.2(3) . . ? N10 Ni1 N6 92.3(3) . . ? N9 Ni1 N6 166.1(4) . . ? N5 Ni1 N6 76.5(3) . . ? N8 Ni2 N12 92.1(3) . . ? N8 Ni2 N4 95.3(3) . . ? N12 Ni2 N4 94.5(4) . . ? N8 Ni2 N11 164.4(3) . . ? N12 Ni2 N11 77.1(3) . . ? N4 Ni2 N11 96.8(3) . . ? N8 Ni2 N7 78.0(3) . . ? N12 Ni2 N7 90.0(3) . . ? N4 Ni2 N7 172.0(3) . . ? N11 Ni2 N7 90.7(3) . . ? N8 Ni2 N3 90.3(3) . . ? N12 Ni2 N3 172.3(3) . . ? N4 Ni2 N3 78.1(4) . . ? N11 Ni2 N3 101.8(3) . . ? N7 Ni2 N3 97.6(3) . . ? C5 N1 C1 115.5(10) . . ? C5 N1 Ni1 116.7(7) . . ? C1 N1 Ni1 127.6(8) . . ? C6 N2 C7 114.6(8) . . ? C6 N2 Ni1 113.8(6) . . ? C7 N2 Ni1 131.6(7) . . ? C19 N3 C16 118.0(9) . . ? C19 N3 Ni2 114.1(7) . . ? C16 N3 Ni2 127.5(6) . . ? C24 N4 C20 117.5(10) . . ? C24 N4 Ni2 129.6(9) . . ? C20 N4 Ni2 112.8(8) . . ? C25 N5 C29 119.8(9) . . ? C25 N5 Ni1 125.2(8) . . ? C29 N5 Ni1 114.9(7) . . ? C30 N6 C31 117.3(9) . . ? C30 N6 Ni1 110.4(7) . . ? C31 N6 Ni1 131.9(6) . . ? C43 N7 C40 119.5(9) . . ? C43 N7 Ni2 112.0(7) . . ? C40 N7 Ni2 127.6(6) . . ? C48 N8 C44 115.2(9) . . ? C48 N8 Ni2 130.6(8) . . ? C44 N8 Ni2 114.3(6) . . ? C53 N9 C49 116.5(10) . . ? C53 N9 Ni1 117.0(8) . . ? C49 N9 Ni1 126.4(7) . . ? C54 N10 C55 115.7(8) . . ? C54 N10 Ni1 113.6(7) . . ? C55 N10 Ni1 130.7(6) . . ? C67 N11 C64 115.0(8) . . ? C67 N11 Ni2 112.9(7) . . ? C64 N11 Ni2 131.6(6) . . ? C68 N12 C72 120.6(10) . . ? C68 N12 Ni2 113.4(7) . . ? C72 N12 Ni2 125.8(8) . . ? C2 C1 N1 121.2(11) . . ? C3 C2 C1 123.5(12) . . ? C2 C3 C4 116.1(12) . . ? C5 C4 C3 116.8(11) . . ? N1 C5 C4 126.6(10) . . ? N1 C5 C6 113.5(10) . . ? C4 C5 C6 119.6(10) . . ? N2 C6 C5 118.3(9) . . ? C12 C7 C8 118.3(10) . . ? C12 C7 N2 120.2(10) . . ? C8 C7 N2 120.9(8) . . ? C9 C8 C7 120.0(10) . . ? C10 C9 C8 121.4(12) . . ? C9 C10 O1 118.7(10) . . ? C9 C10 C11 120.2(11) . . ? O1 C10 C11 120.2(10) . . ? C12 C11 C10 118.6(12) . . ? C7 C12 C11 120.7(12) . . ? C14 C13 O1 120.3(11) . . ? C14 C13 C18 119.6(12) . . ? O1 C13 C18 120.0(10) . . ? C13 C14 C15 120.5(11) . . ? C16 C15 C14 119.9(10) . . ? C15 C16 C17 118.9(10) . . ? C15 C16 N3 118.4(9) . . ? C17 C16 N3 122.6(10) . . ? C18 C17 C16 121.8(12) . . ? C17 C18 C13 119.1(11) . . ? N3 C19 C20 121.2(11) . . ? C21 C20 N4 120.5(13) . . ? C21 C20 C19 125.9(14) . . ? N4 C20 C19 113.5(11) . . ? C20 C21 C22 118.9(16) . . ? C23 C22 C21 116.4(14) . . ? C24 C23 C22 122.4(17) . . ? C23 C24 N4 124.0(15) . . ? N5 C25 C26 122.7(12) . . ? C25 C26 C27 115.3(13) . . ? C28 C27 C26 120.6(14) . . ? C29 C28 C27 119.9(13) . . ? N5 C29 C28 121.6(10) . . ? N5 C29 C30 115.0(10) . . ? C28 C29 C30 123.3(11) . . ? N6 C30 C29 123.1(10) . . ? C36 C31 C32 121.3(10) . . ? C36 C31 N6 120.8(10) . . ? C32 C31 N6 117.7(9) . . ? C31 C32 C33 119.0(11) . . ? C32 C33 C34 119.7(11) . . ? C35 C34 O2 120.3(10) . . ? C35 C34 C33 120.5(10) . . ? O2 C34 C33 119.1(10) . . ? C34 C35 C36 120.6(11) . . ? C31 C36 C35 118.6(10) . . ? C38 C37 C42 121.2(9) . . ? C38 C37 O2 117.9(10) . . ? C42 C37 O2 120.8(9) . . ? C37 C38 C39 121.3(10) . . ? C38 C39 C40 119.2(9) . . ? C41 C40 N7 120.1(10) . . ? C41 C40 C39 118.3(9) . . ? N7 C40 C39 121.5(9) . . ? C40 C41 C42 121.3(10) . . ? C41 C42 C37 118.6(9) . . ? N7 C43 C44 122.4(10) . . ? C45 C44 N8 123.9(10) . . ? C45 C44 C43 123.6(11) . . ? N8 C44 C43 112.4(9) . . ? C46 C45 C44 118.1(13) . . ? C45 C46 C47 121.4(13) . . ? C46 C47 C48 116.4(12) . . ? N8 C48 C47 125.0(13) . . ? C50 C49 N9 120.9(13) . . ? C49 C50 C51 119.9(13) . . ? C52 C51 C50 119.3(13) . . ? C51 C52 C53 115.8(13) . . ? N9 C53 C52 127.3(12) . . ? N9 C53 C54 115.1(11) . . ? C52 C53 C54 117.6(11) . . ? N10 C54 C53 116.8(10) . . ? C56 C55 C60 118.3(10) . . ? C56 C55 N10 119.9(9) . . ? C60 C55 N10 121.7(9) . . ? C55 C56 C57 122.0(11) . . ? C58 C57 C56 119.9(10) . . ? C57 C58 C59 119.9(10) . . ? C57 C58 O3 124.0(8) . . ? C59 C58 O3 116.1(9) . . ? C58 C59 C60 120.5(10) . . ? C55 C60 C59 119.4(10) . . ? C66 C61 C62 121.3(11) . . ? C66 C61 O3 119.6(11) . . ? C62 C61 O3 119.0(10) . . ? C63 C62 C61 117.9(11) . . ? C62 C63 C64 122.2(12) . . ? C65 C64 C63 119.0(11) . . ? C65 C64 N11 119.3(9) . . ? C63 C64 N11 121.7(10) . . ? C64 C65 C66 121.0(12) . . ? C61 C66 C65 118.6(13) . . ? N11 C67 C68 119.2(9) . . ? C13 O1 C10 116.8(8) . . ? C34 O2 C37 119.0(8) . . ? C58 O3 C61 113.5(8) . . ? N12 C68 C69 122.9(10) . . ? N12 C68 C67 117.1(10) . . ? C69 C68 C67 120.0(10) . . ? C70 C69 C68 118.1(12) . . ? C71 C70 C69 116.5(13) . . ? C70 C71 C72 122.2(12) . . ? N12 C72 C71 119.3(11) . . ? F14' B1 F14 44.4(17) . . ? F14' B1 F13' 106(2) . . ? F14 B1 F13' 128.2(19) . . ? F14' B1 F11 127.5(11) . . ? F14 B1 F11 128.8(10) . . ? F13' B1 F11 102.9(17) . . ? F14' B1 F12' 91.6(18) . . ? F14 B1 F12' 48.1(12) . . ? F13' B1 F12' 135.7(13) . . ? F11 B1 F12' 96.8(9) . . ? F14' B1 F12 116.9(12) . . ? F14 B1 F12 109.6(11) . . ? F13' B1 F12 36.1(11) . . ? F11 B1 F12 112.5(8) . . ? F12' B1 F12 99.7(9) . . ? F14' B1 F13 38.3(14) . . ? F14 B1 F13 81.6(14) . . ? F13' B1 F13 90.2(14) . . ? F11 B1 F13 100.3(9) . . ? F12' B1 F13 124.8(11) . . ? F12 B1 F13 120.4(10) . . ? B1 F13 F14 49.0(7) . . ? B1 F14 F13 49.3(8) . . ? F22 B2 F24 116.8(15) . . ? F22 B2 F22' 30.2(13) . . ? F24 B2 F22' 125.9(15) . . ? F22 B2 F24' 88.8(16) . . ? F24 B2 F24' 30.7(13) . . ? F22' B2 F24' 95.4(15) . . ? F22 B2 F23 124.4(15) . . ? F24 B2 F23 110.5(15) . . ? F22' B2 F23 97.2(14) . . ? F24' B2 F23 124.5(14) . . ? F22 B2 F23' 133.9(15) . . ? F24 B2 F23' 92.6(15) . . ? F22' B2 F23' 103.9(15) . . ? F24' B2 F23' 105.7(16) . . ? F23 B2 F23' 19.1(17) . . ? F22 B2 F21 90.6(12) . . ? F24 B2 F21 97.7(13) . . ? F22' B2 F21 114.9(12) . . ? F24' B2 F21 112.0(12) . . ? F23 B2 F21 110.6(10) . . ? F23' B2 F21 121.4(14) . . ? F32' B3 F31 124.7(13) . . ? F32' B3 F33' 109.9(10) . . ? F31 B3 F33' 80.7(13) . . ? F32' B3 F34 61.4(11) . . ? F31 B3 F34 109.5(11) . . ? F33' B3 F34 48.5(9) . . ? F32' B3 F31' 109.1(11) . . ? F31 B3 F31' 29.0(13) . . ? F33' B3 F31' 109.4(11) . . ? F34 B3 F31' 127.0(11) . . ? F32' B3 F34' 110.7(12) . . ? F31 B3 F34' 116.3(10) . . ? F33' B3 F34' 109.2(12) . . ? F34 B3 F34' 123.9(11) . . ? F31' B3 F34' 108.5(9) . . ? F32' B3 F32 127.5(14) . . ? F31 B3 F32 107.8(10) . . ? F33' B3 F32 77.4(14) . . ? F34 B3 F32 104.5(13) . . ? F31' B3 F32 117.1(11) . . ? F34' B3 F32 32.1(14) . . ? F32' B3 F33 39.4(11) . . ? F31 B3 F33 112.1(12) . . ? F33' B3 F33 149.0(10) . . ? F34 B3 F33 100.8(10) . . ? F31' B3 F33 85.0(12) . . ? F34' B3 F33 90.7(13) . . ? F32 B3 F33 121.2(14) . . ? F44' B4 F43 132.0(14) . . ? F44' B4 F44 61.9(13) . . ? F43 B4 F44 104.2(14) . . ? F44' B4 F41 113.3(9) . . ? F43 B4 F41 114.3(12) . . ? F44 B4 F41 99.0(13) . . ? F44' B4 F42' 125.0(14) . . ? F43 B4 F42' 43.8(12) . . ? F44 B4 F42' 145.6(13) . . ? F41 B4 F42' 106.0(10) . . ? F44' B4 F42 54.3(12) . . ? F43 B4 F42 115.3(16) . . ? F44 B4 F42 116.2(14) . . ? F41 B4 F42 106.9(11) . . ? F42' B4 F42 78.8(13) . . ? F44' B4 F43' 98.9(14) . . ? F43 B4 F43' 53.2(12) . . ? F44 B4 F43' 51.0(10) . . ? F41 B4 F43' 116.6(13) . . ? F42' B4 F43' 96.0(12) . . ? F42 B4 F43' 135.8(14) . . ? N13 C73 C74 178(3) . . ? N14 C75 C76 172(4) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.317 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.069 #### END of this CIF #### ######################################################################## #### END of All #### #######################################################################